CN103822961A - Electrochemical microfluidic chip and preparation method thereof - Google Patents
Electrochemical microfluidic chip and preparation method thereof Download PDFInfo
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- CN103822961A CN103822961A CN201410092148.2A CN201410092148A CN103822961A CN 103822961 A CN103822961 A CN 103822961A CN 201410092148 A CN201410092148 A CN 201410092148A CN 103822961 A CN103822961 A CN 103822961A
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Abstract
The invention discloses an electrochemical microfluidic chip which comprises a metal Cr layer arranged on a substrate, wherein a metal Au layer is arranged on the metal Cr layer, a metal Bi layer serving as a working electrode and an electrode Ag or AgCl layer serving as an auxiliary electrode are arranged on the metal Au layer, an upper cover is arranged on the substrate, and a gap between the upper cover and the substrate is a microfluidic channel. According to the electrochemical microfluidic chip and a preparation method thereof, the chip of a portable on-line water ion detection instrument based on an electrochemical stripping method is prepared with an MEMS (micro-electro-mechanical system) microfabrication technology, and preparation of an electrochemical microfluidic chip unit can be finished only by a common ultraviolet light source and a common mask template by aid of the excellent high-precision structural forming capacity of photoresist. The electrochemical microfluidic chip is simple in technology and low in cost, and batch production is facilitated.
Description
Technical field
The present invention relates to a kind of to residual galvanochemistry micro flow chip of heavy metal ion, negative ion, agricultural chemicals, pesticide, medicine, cosmetics and articles for washing etc. in water and preparation method thereof, in particular to the micro-fluidic detection chip of a kind of galvanochemistry of preparing based on micro-nano process technology and manufacture method thereof.
Background technology
Along with socioeconomic fast development, water body comprises river, river, lake, sea and underground water intermediate ion, comprises that heavy metal cation and anion concentration also constantly raise.Because development pattern is extensive, pollute long-term accumulated, the relevant harmful toxic matter such as some basin Regional Gravity And metals pollutes very outstanding, and particularly mercury, chromium, cadmium, lead, the heavy metal pollution of arsenic class highlight.The harmful toxic matter such as heavy metal pollutes and causes taking place frequently of drinking water pollution accident, require us must strengthen improvement and control and monitoring that the harmful toxic matters such as heavy metal are polluted, set up comprehensive monitoring and early warning system, to eliminate the harm to ecological environment security and drinking water safety.
At present, the detection of these ions is also rested on to spot sampling, deliver to the conventional program that laboratory is detected.This not only can not grasp the information of object ion concentration change and distribution in time, gets its migration and variation rule in environment clear, provides foundation accurately to formulating the policy of corresponding pollution abatement.And the impact of various factors tends to change form and the concentration of sample component in sample collection, storage, transportation.
At present the detection method of heavy metal ion is had to atomic absorption spectrography (AAS) (AAS), atom fluorescent luminosity method (AFS), inductive coupling emission spectrometry (ICP-AES), inductive coupling mass spectroscopy (ICP-MS) and the chromatography of ions etc.In these methods, AAS and AFS need the heavy metal ion in solution to be gasificated into gas atom form (temperature approximately 1,000K-1,500K), again by measure its absorbance log (AAS) to resonance absorption light or be stimulated after the wavelength of fluorescence that gives off, and intensity (AFS) is carried out quantitative and qualitative analysis calculating.ICP method more will be heated as heavy metal ion plasma (temperature reaches 10,000K), then records atomic emission spectrum (AES) or carry out mass-spectrometer measurement and carry out qualitative and quantitative analysis.AAS, AFS and ICP method, detectability is at 10-7-10-10mol/L, the range of linearity wide (3-5 the order of magnitude), precision is high, except AAS can carry out multielement and Determination of Different Valence States.But the instrument operation expense of these methods is high, and analysis time is long, can not carry out field quick detection.The chromatography of ions, is to utilize the different different exchange capacities of ion pair ion exchange resin to separate different ions, leads or ultraviolet-visible spectrophotometer detects in electricity consumption, can separate detection different kinds of ions simultaneously.Sample needs pre-service (filter, extraction, saltouts etc.), and the manufacture of separating column requires higher.
Electrochemical Stripping voltammetry is considered to detect the effective method the most of water body intermediate ion, especially heavy metal ion always.Portable water ion on-line detector based on Electrochemical Stripping Analysis, can realize the scene to above-mentioned Heavy Metals in Waters ion and some negative ion, online, fast detecting.
Electrochemical Stripping analytic approach is in solution, to have different electrochemical properties according to different band electron ion, by the electric current of measuring the electromotive force in oxidation/reduction process and producing, carries out qualitative, quantitative method.That current generally acknowledged one is quick, accurately, sensitive analytical approach.Because instrument equipment is simple, be easy to operately easy to miniaturization.And Electrochemical Detection unit is also detection chip, be the core of Electrochemical Stripping analytic approach, it completes the measurement of the enrichment to ion, electrolysis stripping and current potential, electric current in the lump.
Summary of the invention
The object of the invention is to overcome the above problem that prior art exists, a kind of galvanochemistry micro flow chip and preparation method thereof is provided, overcome the deficiency of the detecting instrument of existing heavy metal ion, portable water ion on-line detector principle of work based on Electrochemical Stripping Analysis, utilize MEMS processing (photoetching, sputter, electroplate) technology, on polymkeric substance COC substrate, prepare a kind of portable water ion on-line detector chip based on Electrochemical Stripping Analysis, through Accurate Calibration, make it meet heavy metal, negative ion, agricultural chemicals, pesticide, medicine, cosmetics, wait on-line testing requirement with articles for washing etc. is residual.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the present invention is achieved through the following technical solutions:
A kind of galvanochemistry micro flow chip, comprise and be arranged on suprabasil Metal Cr layer, on described Metal Cr layer, be provided with metal A u layer, on described metal A u layer, be provided with as the metal Bi layer of working electrode with as Electrode Ag or the AgCl layer of auxiliary electrode, in described substrate, be provided with upper cover, the space between upper cover and substrate is fluid channel.
Preferably, described substrate is cyclenes copolymer material.
Preferably, described fluid channel is cyclenes copolymer material.
Preferably, described upper cover is strip, and middle part is wider than two ends, and two ends are fillet, and upper cover center is the groove that holds described galvanochemistry micro flow chip.
A preparation method for galvanochemistry micro flow chip, comprises the following steps:
In step 1) COC substrate, splash-proofing sputtering metal Cr layer, metal A u layer and metal Bi layer, carry out whirl coating, front baking, section, exposure, middle baking, development treatment successively, according to the electrochemical chip structure of mask design, realizes the graphical of its photoresist structure;
Step 2) with the method for solution etching, etch metal electrode Au and working electrode metal Bi layer;
Step 3) is electroplated out Electrode Ag or AgCl layer with electro-plating method;
Step 4), with injection molding forming method, produces the fluid channel of cyclenes copolymer material;
Then step 5) in the gluing mode connecing of ultra-violet curing, encapsulates electrode base sheet and fluid channel.
The invention has the beneficial effects as follows:
The present invention prepares the portable water ion on-line detector chip based on Electrochemical Stripping Analysis with MEMS Micrometer-Nanometer Processing Technology, and only need use general ultraviolet light source, by the high-precision configuration forming ability of photoresist excellence, use common mask, just can complete the preparation of galvanochemistry micro flow chip unit.Technique of the present invention is simple, cost is low, and is easy to mass production.
The present invention can not only be used for water heavy metal and detect, and also can be used for residual etc. the measurement of negative ion, agricultural chemicals, pesticide, medicine, cosmetics, articles for washing.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of instructions, below with preferred embodiment of the present invention and coordinate accompanying drawing to be described in detail as follows.The specific embodiment of the present invention is provided in detail by following examples and accompanying drawing thereof.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide a further understanding of the present invention, forms the application's a part, and schematic description and description of the present invention is used for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is galvanochemistry micro flow chip schematic diagram provided by the invention;
Fig. 2 a is splash-proofing sputtering metal layer Cr layer, Au layer and Bi layer;
Fig. 2 b is etching metal Bi layer;
Fig. 2 c is etching metal A u layer;
Fig. 2 d is electroplated electrode Ag or AgCl layer;
Fig. 2 e removes unnecessary Metal Cr layer;
Fig. 2 f is encapsulation microfluid raceway groove and electrode basement;
Fig. 3 is superstructure schematic diagram.
Wherein: 1, Metal Cr layer, 2, metal A u layer, 3, metal Bi layer, 4, Electrode Ag or AgCl layer, 5, substrate, 6, fluid channel, 7, upper cover.
Embodiment
Below with reference to the accompanying drawings and in conjunction with the embodiments, describe the present invention in detail.
Shown in Fig. 1, a kind of galvanochemistry micro flow chip, comprise the Metal Cr layer 1 being arranged in substrate 5, on described Metal Cr layer 1, be provided with metal A u layer 2, on described metal A u layer 2, be provided with as the metal Bi layer 3 of working electrode with as Electrode Ag or the AgCl layer 4 of auxiliary electrode, in described substrate 5, be provided with upper cover 7, the space between upper cover 7 and substrate 5 is fluid channel 6.Described substrate 5 and fluid channel 6 are cyclenes copolymer material.Shown in Fig. 3, described upper cover 7 is strip, and middle part is wider than two ends, and two ends are fillet, and upper cover 7 centers are the groove that holds described galvanochemistry micro flow chip.
Shown in Fig. 2 a to Fig. 2 f, the present embodiment is implemented under following implementation condition and technical requirement condition:
(1) clean.Three inches of cyclenes copolymers (COC) are substrate 5, and acetone, ethanol, deionized water respectively clean 5 minutes, dry up with nitrogen afterwards, are placed in super-clean environment.
(2), in the COC substrate 5 of 3 inches, the Metal Cr layer 1 that in the COC substrate 5 after cleaning up, first sputter a layer thickness is 20-50nm is as articulamentum.
(3) metal A u layer 2 sputter.On the Metal Cr layer 1 of sputter, the golden film that sputter a layer thickness is 100-200nm.
(4) metal Bi layer 3 sputter.On the metal A u of sputter layer 2, then sputter a layer thickness bismuth film that is 100-150nm.
(5) graphical Bi electrode.On the metal Bi of sputter layer 3, utilize the steps such as gluing, exposure and development in MEMS technique, figure dissolves metal Bi electrode pattern.
(6) metal Bi layer 3 etching.Utilize metal Bi etching solution, remove unnecessary metal Bi, then remove unnecessary photoresist.
(7) graphical Au electrode.On metal Bi layer 3 after etching, utilize the steps such as gluing, exposure and development in MEMS technique, figure dissolves metal A u electrode pattern.
(8) metal A u layer 2 etching.Utilize metal A u etching solution, remove unnecessary metal A u, then remove unnecessary photoresist.
(9) patterned electrodes Ag or AgCl layer 4.On metal A u layer 2 after etching, utilize the steps such as gluing, exposure and development in MEMS technique, figure dissolves metal A g or AgCl electrode pattern.
(10) Electrode Ag or AgCl layer 4 are electroplated.In the silver-colored electroplating solution configuring, carry out the plating of Ag or AgCl electrode.
(11) prepared by fluid channel 6.Utilize injection molding technology, prepare the microfluid raceway groove with the micro-base material of COC.
(12) encapsulation.Utilize ultra-violet curing glue, the telephoning telephony test electrode substrate preparing and fluid channel 6 are encapsulated, form electro-chemical test chip.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. a galvanochemistry micro flow chip, it is characterized in that: comprise the Metal Cr layer (1) being arranged in substrate (5), on described Metal Cr layer (1), be provided with metal A u layer (2), on described metal A u layer (2), be provided with as the metal Bi layer (3) of working electrode with as Electrode Ag or the AgCl layer (4) of auxiliary electrode, in described substrate (5), be provided with upper cover (7), the space between upper cover (7) and substrate (5) is fluid channel (6).
2. galvanochemistry micro flow chip according to claim 1, is characterized in that: described substrate (5) is cyclenes copolymer material.
3. galvanochemistry micro flow chip according to claim 1, is characterized in that: described fluid channel (6) is cyclenes copolymer material.
4. galvanochemistry micro flow chip according to claim 1, is characterized in that: described upper cover (7) is strip, and middle part is wider than two ends, and two ends are fillet, and upper cover (7) center is the groove that holds described galvanochemistry micro flow chip.
5. a preparation method for galvanochemistry micro flow chip, is characterized in that, comprises the following steps:
In the substrate of step 1) cyclenes copolymer, splash-proofing sputtering metal Cr layer, metal A u layer and metal Bi layer, carry out successively whirl coating, front baking, section, exposure, middle baking, development treatment, according to the electrochemical chip structure of mask design, realize the graphical of its photoresist structure;
Step 2) with the method for solution etching, etch metal electrode Au and working electrode metal Bi layer;
Step 3) is electroplated out Electrode Ag or AgCl layer with electro-plating method;
Step 4), with injection molding forming method, produces the fluid channel of cyclenes copolymer material;
Then step 5) in the gluing mode connecing of ultra-violet curing, encapsulates electrode base sheet and fluid channel.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105717166A (en) * | 2016-02-15 | 2016-06-29 | 江苏大学 | Tree growth state real-time detecting device and method based on micro-fluidic chip |
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| CN101603938A (en) * | 2008-06-11 | 2009-12-16 | 中山大学 | Be used for micro-nano structure bismuth pole of trace heavy metal detection and preparation method thereof |
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| CN105717166A (en) * | 2016-02-15 | 2016-06-29 | 江苏大学 | Tree growth state real-time detecting device and method based on micro-fluidic chip |
| CN105717166B (en) * | 2016-02-15 | 2019-08-27 | 江苏大学 | A kind of arboreal growth real-time detection device for state and method based on micro-fluidic chip |
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