CN102519907B - Reflection type refractive index sensor based on optical fibre and micro-fluidic chip - Google Patents

Reflection type refractive index sensor based on optical fibre and micro-fluidic chip Download PDF

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CN102519907B
CN102519907B CN201110423100.1A CN201110423100A CN102519907B CN 102519907 B CN102519907 B CN 102519907B CN 201110423100 A CN201110423100 A CN 201110423100A CN 102519907 B CN102519907 B CN 102519907B
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optical fibre
channel
micro
optical
passage
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CN102519907A (en
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张磊
方伟
童利民
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Zhejiang University ZJU
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Abstract

The invention discloses a reflection type refractive index sensor based on an optical fibre and a micro-fluidic chip, wherein a detection channel, an incidence optical fibre channel and an exit optical fibre channel are arranged on the micro-fluidic chip; the incidence optical fibre channel and the exit optical fibre channel are arranged at the same side of the detection channel; a light exit hole of the incidence optical fibre channel and a light incidence hole of the exit optical fibre channel are mutually spaced with the detection channel; furthermore, after being reflected by the side wall of the detection channel, light exited from the incidence optical fibre channel can be incident in the exit optical fibre channel; the optical fibre is matched with the optical fibre channels; the end face of the optical fibre is aligned to the end faces of the optical fibre channels; and the optical fibre is connected with an external light source and a light intensity detector through a standard interface. A refractive index detection range of the sensor can be adjusted by changing an included angle between the exit optical fibre channel and the detection channel. Because of reflective detection, the sensor can be used for detecting non-transparent liquid samples, thus, the sensor disclosed by the invention is capable of realizing refractive index measurement of micro-liquid samples in different refractive index ranges.

Description

Reflection-type optical fiber-micro-fluidic chip index sensor
Technical field
The present invention relates to the sensor based on optical fiber and micro-fluidic chip, particularly relate to the micro liquid biochemical sensor that refractive index detects.
Background technology
Micro-fluidic chip is one of current scientific research hot fields, has broad prospect of application in fields such as life science, chemistry, optics.Because micro-fluidic chip passage yardstick can reduce sample consumption tens of to hundreds of micron dimensions conventionally greatly, improve level of integrated system.The micro-fluidic chip optical sensor using at present relies on complicated light path system or accurate process technology conventionally, thereby has seriously limited its practical application in fields such as clinical diagnose, environmental monitoring and food securities.
Refractive index is a kind of conventional index that detects, and is generally used for the sample detection, the detection of for example sucrose concentration and the unmarked biology sample detection that do not have fluorescence and characteristic light to absorb.The portable refractive index detecting instrument of now widely used commercialization adopts prism as detecting element more, shows refractive index value by eyepiece people for reading refractive index value or instrument, and the sensitivity of the refractive index detecting instrument of this type is conventionally 10 -3-10 -4refractive index unit's magnitude.Its refractive index sensitivity of surface plasma body resonant vibration (SPR) analyser using in life science can reach 10 -6more than refractive index unit's magnitude, but its price is very expensive, and volume is larger, high to sample requirement, is difficult to adapt to the demand of field quick detection.
Mostly the micro-fluidic chip index sensor of report is integrated resonator cavity or micro-machined interferometer on micro-fluidic chip at present, by the mobile message at measure spectrum peak, obtains the refractive index of sample.Typical example comprises micro-ring resonant cavity prepared by micro-nano fiber and the integrated index sensor of micro-fluidic chip; The index sensor that micro-machined Mach-Zehnder interferometer and micro-fluidic chip are integrated etc.Sensors with auxiliary electrode were not only needs expensive process equipment and complicated process, and is difficult to the consistance of the performance that ensures each sensor, the more important thing is that its sensitivity depends on the resolution of external spectrometer.
Be another approach that detects refractive index by measuring light intensity variation, the micro-nano fiber micro-fluidic chip index sensor of such as embedding formula and optical fiber draw the most advanced and sophisticated index sensor of cone etc.The variation of sample refractive index will cause that the peripheral evanscent field of micro-nano fiber or optical fiber draw the variation of the most advanced and sophisticated optical field distribution of cone, thereby causes the change of output intensity signal.This class sensor does not need to depend on expensive high-resolution spectrometer, and detection sensitivity can reach 10 -4refractive index unit's magnitude.But the subtle change of the most advanced and sophisticated profile of micro-nano fiber diameter or tapered fiber, can cause the marked change of index sensor performance, thereby make the sensor of this type be difficult to use in industrialized large-scale production.
In the recent period, research worker's a kind of continuously adjustable optical attenuator of having reported for work, this attenuator uses a standard fiber that incident light is introduced to micro-fluidic chip, after lenticule group collimation, there is reflection and refraction at interface, microchannel in light, reflected light is injected an outgoing optical fiber through another lens combination, by regulating the refractive index of solution in microchannel, the output intensity of outgoing optical fiber changes thereupon.If this optical attenuator is directly used and has two defects as index sensor: first, incident angle can only be corresponding the sensitizing range of 0.01-0.02 refractive index unit, for example, in the time that incident angle is 69 °, the solution variations in refractive index sensitivity of a sensor refractive index within the scope of 1.33-1.34; The second, on micro-fluidic chip, integral micro-lens needs expensive process equipment, and processing cost is high.
Therefore, study a kind of micro-fluidic chip index sensor simple in structure, that refractive index sensing range is wide all significant for the research and development in the fields such as life science, environmental monitoring and food quality control.
Summary of the invention
One of object of the present invention is to provide a kind of reflection-type optical fiber-micro-fluidic chip index sensor simple in structure.
Two of object of the present invention is to provide the continuously adjustable reflection-type optical fiber-micro-fluidic chip of a kind of refractive index sensing range index sensor.
For realizing above object, the technical solution used in the present invention is: this reflection-type optical fiber-micro-fluidic chip index sensor comprises the micro-fluidic chip of being made up of transparent material, the inside of micro-fluidic chip is provided with sense channel, be provided with incident optical passage and outgoing optical-fibre channel in the same side of sense channel, the beam projecting mouth of incident optical passage, the light entrance port of outgoing optical-fibre channel, sense channel space, and after the sidewall reflects of passage, can be incided in outgoing optical-fibre channel after testing by the light of incident optical passage outgoing, optical fiber in incident optical passage and outgoing optical-fibre channel matches with passage separately, the end face of the beam projecting mouth of the end face of the exit end of the optical fiber in incident optical passage and incident optical passage, the end face of the end face of the incident end of the optical fiber in outgoing optical-fibre channel and the light entrance port of outgoing optical-fibre channel.
Preferably, the present invention can be incided the sidewall reflects of passage more than one in outgoing optical-fibre channel after testing from the light of same incident optical passage outgoing.
Preferably, the described sidewall of sense channel of the present invention is perpendicular to the bottom surface of this sense channel.
Preferably, the xsect of sense channel of the present invention is rectangular.
Compared with prior art, the invention has the beneficial effects as follows: (1) is known according to fresnel formula, in the time there is transmitting and refraction at the interface of the different material of two kinds of refractive indexes in light, different refractive index sensitive range corresponding to incident angle.The present invention is not in the situation that carrying out lenticule collimation to light, and the optical fiber by incident ray in incident optical passage is with the sidewall of certain angle of divergence directive sense channel, thereby obtained one group of incident angle continually varying incident ray; And incident ray is loose through the follow-up supervention of sidewall reflects of sense channel, therefore, just can collect by the optical fiber in the catoptrical outgoing optical-fibre channel of one or more collections of different reflection angle settings the reflection ray that different incident raies produce, thereby realize, the refractive index of different refractivity scope sample solution be detected.(2) sensor of the present invention can use standard commercial optical fiber, can with peripheral light source, light intensity detector slitless connection, realize detect in real time and hazardous environment under remote recording, and can avoid the use of expensive high resolution spectrometer.(3) sensor construction of the present invention is simple, without integral micro-lens, does not therefore need to use expensive process equipment, and process is simple and processing cost is low, and the favorable repeatability of sensor, is convenient to large-scale production.
Brief description of the drawings
Fig. 1 is the structural representation that the present invention has reflection-type optical fiber-micro-fluidic chip index sensor of an incident optical passage and a corresponding outgoing optical-fibre channel;
Fig. 2 is the structural representation that the present invention has reflection-type optical fiber-micro-fluidic chip index sensor of an incident optical passage and three outgoing optical-fibre channels;
Fig. 3 is that sensor of the present invention is in the time that the emergence angle of light is 69 °, by the measured refractometry working curve of different refractivity ethylene glycol solution introducing sense channel;
Fig. 4 is that sensor of the present invention is in the time that the emergence angle of light is respectively 71 °, 72 °, 74 °, by the measured refractometry working curve of different refractivity ethylene glycol solution introducing sense channel.
In figure: 1-PDMS substrate, 2-sheet glass substrate, 3-sense channel, 4-incident optical passage, 5,5-1,5-2-outgoing optical-fibre channel, 6-incident optical, 7,7-1,7-2-outgoing optical fiber, 8-light source, 9-light intensity detector, the solution entrance of 10-sense channel, the taphole of 11-sense channel, the echo area of 12-sense channel, the beam projecting mouth of 13-incident optical passage, the light entrance port of 14-outgoing optical-fibre channel, the optical fiber insert port of 15-incident optical passage, outgoing optical-fibre channel.
Embodiment
Make micro-fluidic chip and use commercial single-mode fiber (125 microns of external diameters, 10 microns of core diameters) that structure of sensor of the present invention and preparation method thereof is described for example with transparent polymer dimethyl silicone polymer (PDMS) below.It should be noted that, this embodiment is not the restriction to technical solution of the present invention, the present invention also can use other transparent materials make micro-fluidic chip and use other optical fiber, the size numerical value relevant with optical fiber with each passage is only for explanation the present invention's convenience is used, and is not limited to following lifted concrete numerical value.
Specifically, micro-fluidic chip can adopt SU-8 formpiston and refractive index to be about 1.41 PDMS to be prepared.First according to the ranges of indices of refraction of the refractive index of PDMS and sample, calculate the corresponding reflection coefficient of light of the different incidence angles penetrating through incident optical passage 4 according to fresnel formula as follows:
(1)
(2)
(3)
Wherein, the incident angle that θ is light, n 1for the refractive index of micro-fluidic chip material, n 2for the refractive index of sample, r sfor s wave amplitude reflection coefficient, r pfor p wave amplitude reflection coefficient, for the reflection coefficient of incident ray.
When variations in refractive index is identical, reflection coefficient changes greatly, and refractive index detection sensitivity is higher.Therefore, by calculating reflection coefficient corresponding to different light rays incident angle, can optimize the interval corresponding angle of incidence of light θ of different refractivity, thereby obtain the angle of incident optical passage 4 and outgoing optical-fibre channel 5 and sense channel 3, determine the structure of sensor of the present invention.Then, the structure of the sensor processing SU-8 formpiston according to the present invention.
In sensor of the present invention, sense channel 3 utilizes itself and incident optical passage 4 and the outgoing optical-fibre channel 5 sidewall reflects light in the same side; And the effect of incident optical passage 4 and outgoing optical-fibre channel 5 is fixed fibers, the optical fiber in incident optical passage 4 and outgoing optical-fibre channel 5 is respectively used to outgoing and collects light.The present invention is not particularly limited the shape of cross section of each passage, can be rectangle, triangle, trapezoidal, circular etc.But for sense channel 3 in order to by the light reflection by 4 outgoing of incident optical passage to for the sidewall in outgoing optical-fibre channel 5, as the preferred embodiment of the present invention, this sidewall, perpendicular to the bottom surface of sense channel 3, can ensure that light reflects in same plane like this; Further, the xsect of sense channel 3 is preferably rectangle.And in the time that the xsect of incident optical passage 4 and outgoing optical-fibre channel 5 is rectangle, in technique, easily guarantee that fiber end face flushes with channel end surface.And, SU-8 formpiston is being added to man-hour, with respect to other shape, the xsect of each passage is processed as to rectangle more simple.
When processing SU-8 formpiston, on SU-8 formpiston corresponding to the bossing of sense channel 3, incident optical passage 4 and outgoing optical-fibre channel 5 bottom surface perpendicular to formpiston, thereby the xsect that ensures sense channel 3 is rectangle, and the xsect of incident optical passage 4 and outgoing optical-fibre channel 5 is rectangle.In micro-fluidic chip, propagate in strict accordance with incident and the reflection angle of design in order to ensure light, incident optical passage 4 and outgoing optical-fibre channel 5 should match with the optical fiber inserting wherein respectively, so that insert after incident optical passage 4 and outgoing optical-fibre channel 5 when optical fiber, the optical fiber in passage with respect to channel position fix, not slippage.It is that the commercial single-mode fiber of 125 microns is as incident optical and outgoing optical fiber that the present embodiment adopts external diameter, at this moment (this is other sizes highly also the height (corresponding to the length of rectangular cross section) of bossing corresponding with incident optical passage and outgoing optical-fibre channel SU-8 formpiston can be designed to 130 microns, technician can according to circumstances determine voluntarily, generally, the size of height over width is large), the width width of rectangular cross section (corresponding to) is designed to 125 microns.Because the width of the external diameter of optical fiber in the present embodiment and the bossing corresponding with incident optical passage and outgoing optical-fibre channel is 125 microns, therefore the optical fiber in incident optical passage 4 and outgoing optical-fibre channel 5 can slippage in passage, realizes relatively fixing.
Uncured PDMS is cast on SU-8 formpiston, at the temperature of 85 DEG C, solidify 30 minutes, then itself and SU-8 formpiston are peeled off, formation has the PDMS substrate 1 of sense channel 3, incident optical passage 4 and outgoing optical-fibre channel 5, because PDMS has accurately copied the configuration of SU-8 formpiston, the xsect of each passage is rectangle, and each channel depth is 130 microns, and the width of incident optical passage 4 and outgoing optical-fibre channel 5 is 125 microns.As shown in Figure 1, micro-fluidic chip of the present invention is formed by PDMS substrate 1 and sheet glass substrate 2 bonding after Cement Composite Treated by Plasma with microchannels such as sense channel 3, incident optical passage 4 and outgoing optical-fibre channels 5, and the area of sheet glass substrate 2 is slightly larger than PDMS substrate 1, be beneficial to optical fiber fixing on sheet glass substrate 2.In the present embodiment, can be 1.5 centimetres by the Design of length of sense channel 3, width design be 150 microns (but being not limited to this size), and two ends are respectively equipped with solution entrance 10 and taphole 11; The length of incident optical passage 4 and outgoing optical-fibre channel 5 can design approximately 2 centimetres (but being not limited to this size), incident optical passage 4 and outgoing optical-fibre channel 5 are respectively the beam projecting mouth 13 of incident optical passage 4 and the light entrance port 14 of outgoing optical-fibre channel 5 near one end of sense channel 3, the other end is communicated with micro-fluidic chip is outside, is optical fiber insert port 15.
The protective seam of one section of commercial single-mode fiber 3-4 centimetre is peelled off, then adopted optical fiber cutter that fiber end face is cut smooth; Respectively incident optical smooth end face 6 and outgoing optical fiber 7 are inserted in incident optical passage 4 and outgoing optical-fibre channel 5 through optical fiber insert port 15, and make the end face of the end face of exit end and the beam projecting mouth 13 of incident optical passage 4 of the optical fiber in incident optical passage 4, the end face of the end face of the incident end of the optical fiber in outgoing optical-fibre channel 5 and the light entrance port 14 of outgoing optical-fibre channel 5.Incident optical 6 and outgoing optical fiber 7 are close to sheet glass substrate 2.
Drip uncured PDMS as fluid sealant at optical fiber insert port 15 places, make it infiltrate the gap of optical fiber and optical-fibre channel, at the temperature of 85 DEG C, solidify 30 minutes, the further optical fiber in fixed fiber passage, meanwhile, the incident optical 6 in PDMS substrate 1 outside and outgoing optical fiber 7 are fixed on the surface of sheet glass substrate 2 by PDMS.
While using sensor of the present invention, the optical fiber that is exposed at micro-fluidic chip outside is connected with light source 8 and detector 9 respectively by bare fiber adaptor, adopt the mode of syringe pump injection or negative pressure absorbing to drive solution to flow into sense channel 3 from solution entrance 10, flow out through taphole 11.When solution passes through the echo area 12 of sense channel 3, light intensity detector 9 records the variation of output intensity, realizes the refractive index sensing to sample solution.
Micro-fluidic chip taking reflection angle as the single outgoing optical fiber of 69 ° have further illustrates the technique effect (referring to Fig. 1) of this sensor as example below.
The sensor of the present invention of preparation single outgoing optical fiber as shown in Figure 1, the width of its sense channel 3 is 150 microns, and length is 1.5 centimetres, and the degree of depth is 130 microns.The width of incident optical passage 4 and outgoing optical-fibre channel 5 is 125 microns, and the degree of depth is 130 microns.Incident angle, reflection angle and emergence angle are 69 °.Adopting external diameter is 125 microns, core diameter is about the commercial single-mode fiber of 10 microns as incident optical 6 and the outgoing optical fiber 7 of sensor of the present invention, the helium-neon laser (light source 8) that incident optical 6 is 633nm by bare fiber adaptor with wavelength is connected, and outgoing optical fiber 7 is connected with fiber spectrometer (light intensity detector 9) by bare fiber adaptor.
First 2 microlitre distilled water are dropped in to solution entrance 10, apply negative pressure at taphole 11, make distilled water flow into sense channel 3, and through echo area 12, measure the catoptrical light intensity (I that outgoing optical fiber 7 is exported 0).Then a series of ethylene glycol solutions are introduced respectively to sense channel 3 according to refractive index order from low to high, and measure the catoptrical light intensity (I) that corresponding outgoing optical fiber 7 is exported, calculate catoptrical normalized transmissivity T(T=100% × I/ I that different ethylene glycol solutions are corresponding 0).The working curve of the refractive index of ethylene glycol solution ranges of indices of refraction within the scope of 1.33-1.42 and normalized transmissivity as shown in Figure 3.Be not difficult to find out, in the time that emergence angle is 69 °, the sensitizing range of refractive index is 1.33-1.35.
As the another kind of embodiment of sensor of the present invention, also can be that an incident optical passage is corresponding with plural outgoing optical-fibre channel, make the sidewall reflects of passage 3, can incide in multiple outgoing optical-fibre channels 5 after testing from the light of same incident optical passage 4 outgoing.Further illustrate this continuously adjustable technique effect in sensor refraction rate sensitizing range with the sensor of the present invention of structure shown in Fig. 2 below.In Fig. 2, incident optical passage 4 and three outgoing optical-fibre channels 5,5-1,5-2 are corresponding.
While preparing the sensor of the present invention with 3 outgoing optical fiber as shown in Figure 2, the width that can design sense channel 3 is 150 microns, and length is 1.5 centimetres, and the degree of depth is 130 microns.It is 130 microns that the width of incident optical passage 4 and outgoing optical-fibre channel 5,5-1,5-2 is 125 microns, the degree of depth.The incident angle of incident optical is 71 °, and the reflection angle of outgoing optical fiber 7-1,7,7-2 is respectively 71 °, 72 ° and 74 °.Adopting external diameter is that 125 microns, core diameter are commercial single-mode fiber logical incident optical 6 and outgoing optical fiber 7-1,7, the 7-2 as sensor of the present invention of 10 microns, incident optical 6 is connected with the helium-neon laser (light source 8) taking wavelength as 633nm by bare fiber adaptor, three outgoing optical fiber 7,7-1,7-2 are connected with fiber spectrometer (light intensity detector 9) by bare fiber adaptor successively, measure the information of an outgoing optical fiber at every turn.The ethylene glycol solution refractive index that the 3 kind reflection angle of ranges of indices of refraction within the scope of 1.33-1.42 are corresponding and the working curve of catoptrical normalized transmissivity are as shown in Figure 4.Be not difficult to find out, along with the increase of reflection angle, also move to high index of refraction direction the sensitizing range of refractive index, and have similar sensitivity.Taking reflection angle as the refractive index working curve of 72 ° is as example, in the time that refractive index changes to 1.36 from 1.35, transmission change 70%, refractive index changes at 1.351 o'clock from 1.35, transmission change 30%, its corresponding refractive index sensitivity arrives 3 × 10 -5refractive index unit.Adopt the commercial optical fiber of multimode of 125 microns of diameters to replace the single-mode fiber of 125 microns of diameters also can realize the continuously adjustable technique effect in refractive index sensitizing range, the reflection ray that can collect due to multimode optical fiber has wider reflection angle scope, and the sensitivity of its refractive index is the low order of magnitude of sensitivity as collection optical fiber compared with single-mode fiber.If adopt larger-diameter optical fiber as incident optical and outgoing optical fiber, not only can cause refractive index to reduce, also will cause the size increase of micro-fluidic chip passage, thereby cause the increase of sample consumption.
To sum up, sensor of the present invention simple in structure, refractive index sensitizing range is adjustable continuously, can select different outgoing optical fiber to measure according to different sample ranges of indices of refraction.In addition, the sensitive sensitivity compared with general commercial index sensor of sensor of the present invention has improved 1-2 the order of magnitude, and the actual sample consumption of sensor of the present invention is only number microlitre, from sample consumption and sensitivity, all can meet clinical medical inspection, the needs of environmental monitoring and food safety monitoring.

Claims (4)

1. reflection-type optical fiber-micro-fluidic chip index sensor, it is characterized in that: comprise the micro-fluidic chip of being made by transparent material, the inside of micro-fluidic chip is provided with sense channel (3), be provided with incident optical passage (4) and outgoing optical-fibre channel (5) in the same side of sense channel (3), the beam projecting mouth (13) of incident optical passage (4), the light entrance port (14) of outgoing optical-fibre channel (5), space between sense channel (3), and after the sidewall reflects of passage (3), can be incided in outgoing optical-fibre channel (5) after testing by the light of incident optical passage (4) outgoing, optical fiber in incident optical passage (4) and outgoing optical-fibre channel (5) matches with passage separately, the end face of exit end of optical fiber and the end face of the beam projecting mouth (13) of incident optical passage (4) in incident optical passage (4), the end face of incident end of optical fiber and the end face of the light entrance port (14) of outgoing optical-fibre channel (5) in outgoing optical-fibre channel (5).
2. reflection-type optical fiber-micro-fluidic chip index sensor according to claim 1, is characterized in that: the sidewall reflects of passage (3), can incide in more than one outgoing optical-fibre channel (5) after testing from the light of same incident optical passage (4) outgoing.
3. reflection-type optical fiber-micro-fluidic chip index sensor according to claim 1 and 2, is characterized in that: the described sidewall of described sense channel (3) is perpendicular to the bottom surface of this sense channel (3).
4. want the reflection-type optical fiber-micro-fluidic chip index sensor described in 3 according to right, it is characterized in that: described sense channel (3) xsect rectangular.
CN201110423100.1A 2011-12-16 2011-12-16 Reflection type refractive index sensor based on optical fibre and micro-fluidic chip Expired - Fee Related CN102519907B (en)

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