CN113155760B - Spectrophotometric detection sensor - Google Patents
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Abstract
The spectrophotometric detection sensor comprises a silicon substrate and a glass substrate which are mutually bonded, wherein a detection channel groove is formed in the binding surface of the silicon substrate and is provided with a liquid inlet channel and a liquid outlet channel, a light inlet groove and a light outlet groove are formed in the bottom surface of the silicon substrate, and light transmitting gaps penetrating through the silicon substrate are respectively formed between the starting side of the detection channel groove and the light inlet groove and between the final side of the detection channel groove and the light outlet groove; a light source groove and a reference groove are arranged beside the light inlet groove, and each connecting groove is connected; the light source groove, the reference groove, each connecting groove, the light inlet groove, the light transmitting gap and the detection channel groove start side form a light source light channel cavity, the light outlet groove, the light transmitting gap and the detection channel groove end side form a signal light channel cavity, the two light channel cavities are filled with light waveguides formed by liquid pouring and curing, and the light waveguides form opposite side walls in the detection channel groove; and a detection light source, a reference light source and a photoelectric detector are respectively arranged at the positions of the light source groove, the reference groove and the light outlet groove on the bottom surface of the silicon substrate.
Description
Technical Field
The invention relates to the technical field of spectrophotometry detection and micro-nano sensors, in particular to a spectrophotometry detection sensor.
Background
Quantitative analysis of a substance is performed by measuring the absorbance of light of the substance at a specific wavelength or in a certain range, and this method is called spectrophotometry, also called spectral absorption. The spectrophotometric method is based on Lambert-Beer law, and further obtains the concentration of the measured substance according to the absorbance degree of the measured substance. Method for detecting substances using spectrophotometry: firstly, the detected substances are sampled manually, and different color indicator reagents are added according to different detected substances. When a beam of monochromatic light with a specific wavelength is irradiated into the uniformly mixed solution, spectral absorption is carried out, and the intensity of the absorbed light is in direct proportion to the concentration of the solution. Because the incident light needs to illuminate the liquid under test perpendicularly based on lambert-beer's law.
The specific detection principle relation is as follows:
. Wherein A is the absorbance,
in terms of molar coefficient, L is the thickness of the light-absorbing layer, and c is the concentration of the light-absorbing species.
The initial transmitted light intensity, I is the transmitted light intensity after the indicator is added. In the present invention, the absorbance is measured by the current of the photodiode, and is converted into the relationship between the concentration of the liquid to be measured and the current of the photodiode.
The spectrophotometry has the advantages of good detection precision, short response time, good stability and the like, and the existing spectrophotometry can be used for measuring nutritive salt, turbidity, pH, organic matters, suspended matters and the like, and can be applied to the fields of water quality detection, soil element detection, heavy metal content, food safety and the like. At present, equipment for detecting by using a spectrophotometry method is mainly a spectrophotometer, but the spectrophotometer is large in size and very limited in application scene, and meanwhile, the spectrophotometer can only complete one part of optical detection, so that the integration degree is not high. In addition, there are some hand-held instruments for performing detection by spectrophotometry, which are limited to the measurement of residual chlorine, inorganic salts, etc. and the kinds of measurement are limited, although the volume is reduced more than that of a spectrophotometer.
The micro-nano technology generally refers to nano/micron material, design, manufacture, measurement, control and product technology, and is widely applied to the field of civil products and even military industry. The micro-nano manufacturing technology is an important ring of the micro-nano technology, and currently, the micro-nano manufacturing technology is the most representative silicon micro-processing technology, including the processing of a silicon body and a silicon surface. Silicon micromachining is a technology that serves the production of microelectronics, the main techniques of which include photolithography, thin film growth, dry etching, wet etching, and the like. With the improvement of the requirement of people on the machining precision, the micro-nano technology is a hot point of research at present. Micro-nano sensors are typically associated with MEMS (Micro electro mechanical systems). MEMS refers to high-tech products with dimensions of several millimeters or less, whose internal structures are typically on the order of micrometers or even nanometers, and is an independent intelligent system. The micro-energy-source micro-energy-consumption device mainly comprises a sensor, an actuator and a micro-energy source.
The optical waveguide is a light carrier, and can not only restrict the transmission of light during the transmission process, but also keep the low loss of light during the transmission process. Polymer materials are used to make optical waveguides with the advantages of low dispersion, good substrate compatibility, low absorption coefficient over a wide spectral range, etc. The SU-8 organic polymer material has the advantages of good mechanical property, good filling property, wide controllable range of film thickness and the like, is widely applied to the fields of micro-electro-mechanical systems, micro-flow, packaging, micro-optics and the like, and is a negative, epoxy and near ultraviolet photoresist based on EPON SU-8 resin. At the same time, the SU-8 polymer material has very good optical transparency in the wavelength range of more than 400nm, making it an attractive polymer optical waveguide material.
The micro-nano sensor is a popular direction in the field of sensors in recent years, and the micro-nano sensor field is vigorously supported and developed in China at present. Because a large number of micro device units can be integrated in a small volume space to achieve the purpose of detecting certain physical or chemical quantity, and the mass production can be realized after the scheme is mature, the production and manufacturing cost of the sensor is greatly reduced. The micro-nano sensor is a sensor which is manufactured on semiconductor materials such as silicon or other novel materials by using a micro-scale or nano-scale processing technology as a basis and finally packaged into a whole. The sensor has the technical advantages of small volume, mass production and the like, and the detection precision and range of the sensor can meet most use scenes. The sensor manufactured by the micro-nano technology has the advantages that the size can be made very small on the basis of ensuring the functions, the problem of portability is solved, and the research and application prospects are very wide. However, no reports on the spectrophotometric detection sensor and the manufacturing method thereof are available. Therefore, the inventor of the present application has an idea that a micro-nano manufacturing technology can be used to realize the high integration of sensor components to manufacture a photometric detection sensor which has a small volume and is convenient to carry and can realize field detection.
Disclosure of Invention
The invention aims to solve the technical problem of providing a spectrophotometric detection sensor manufactured by a micro-nano processing technology.
In order to solve the technical problems, the spectrophotometric detection sensor of the invention has the technical scheme that:
the utility model provides a spectrophotometry detection sensor, includes silicon chip and the glass substrate of interbonded, and the glass substrate covers above the silicon chip, the binding face and the bottom surface of silicon chip are the fluting structure that forms through the etching processing, its characterized in that, set up the detection channel groove at silicon chip binding face, the glass substrate has seted up: at least 1 liquid inlet channel communicated with the detection channel groove and used for injecting liquid into the detection channel groove, and at least 1 liquid outlet channel communicated with the detection channel groove and used for discharging liquid outwards; a light inlet groove is formed in the position, corresponding to the starting side of the detection channel groove, of the bottom surface of the silicon substrate, and a light transmitting gap penetrating through the silicon substrate is formed between the starting side of the detection channel groove and the light inlet groove in the bottom surface of the silicon substrate; a light-emitting slot is formed at a position corresponding to the final side of the detection channel slot, and a light-transmitting gap penetrating through the silicon substrate is also formed between the final side of the detection channel slot and the light-emitting slot on the bottom surface of the silicon substrate; a light source groove and a reference groove are formed beside the light inlet groove on the bottom surface of the silicon substrate, the light inlet groove is provided with a connecting groove, and the light source groove and the reference groove are also respectively provided with a connecting groove and connected with the connecting groove of the light inlet groove; the light source groove, the reference groove, the connecting grooves, the light inlet groove and the light transmitting gap form a light source light channel cavity till the starting side of the detection channel groove, the light outlet groove and the light transmitting gap form a signal light channel cavity till the end side of the detection channel groove, the light source light channel cavity and the signal light channel cavity are filled with optical waveguides formed by liquid pouring and curing, and the optical waveguides respectively form opposite side walls at the starting side and the end side of the detection channel groove; and the bottom surface of the silicon substrate is respectively provided with a detection light source, a reference light source and a photoelectric detector for photoelectric conversion at the positions of the light source groove, the reference groove and the light-emitting groove.
The following is a further scheme of the spectrophotometric detection sensor of the present invention:
the side walls of the initial side and the final side of the detection channel groove of the optical waveguide on the silicon substrate binding surface are convex arc-shaped light-gathering walls to form a convex lens shape.
The glass substrate is provided with a liquid to be detected injection through hole and an indicator injection through hole at the corresponding positions of the liquid to be detected interface and the indicator interface respectively; and a merging groove is formed between the to-be-detected liquid interface and the indicator interface, and a mixing channel is formed between the merging groove and the detection channel groove.
The mixing channel is in the shape of an S-shaped travel.
The glass substrate is provided with 2 liquid outlet channels which are communicated with the detection channel grooves and used for discharging liquid outwards, and the liquid outlet channels specifically comprise: the silicon substrate binding surface is respectively provided with 2 waste liquid pools connected with the detection channel groove at the two ends of the detection channel groove, and the glass substrate is respectively provided with 2 waste liquid through holes communicated with the outside at the corresponding positions of the 2 waste liquid pools.
The light source groove and the reference groove are respectively and symmetrically arranged above and below the light inlet groove, and the light source groove, the reference groove and the connection groove are arranged in a Y shape.
The number of the light source grooves is 2, the light source grooves are respectively and symmetrically arranged on the oblique upper side and the oblique lower side of the light inlet groove, and the reference groove is arranged on the outer side of the silicon substrate along the horizontal direction of the connecting groove of the light inlet groove.
The silicon substrate is a rectangular slice block with the same size as the glass substrate, the silicon substrate is a slice block with the thickness of 400 um to 450 um, the slotting depth of the binding face of the silicon substrate is one half of the total thickness of the silicon substrate, the slotting depth of the bottom face of the silicon substrate is one quarter of the total thickness of the silicon substrate, and the depths of the first light-transmitting gap and the second light-transmitting gap are also one quarter of the total thickness of the silicon substrate.
And carrying out oxidation treatment on the inner cavity wall of the molded silicon substrate to form a silicon oxide layer as a light-sparse layer of the internal optical waveguide.
The optical waveguide is made of SU-8 polymer, the detection light source is an LED light emitter or a flashing xenon lamp bare lamp with fixed wavelength, the reference light source is also an LED light emitter or a flashing xenon lamp bare lamp with fixed wavelength, and the photoelectric detector is a photosensitive tube or a photoelectric diode.
The spectrophotometric detection sensor is manufactured by using a single crystal silicon substrate, constructing a required shape on the silicon substrate, using photoresist as an optical waveguide material and then packaging the materials together. Because the processing technology of the silicon substrate is mature at present, and the forming technology of the photoresist as the material of the optical waveguide is also perfect, the spectrophotometric detection sensor with excellent performance and small volume can be prepared in batches, the cost is greatly reduced, and the application scene of the spectrophotometric detection sensor based on the spectrum absorption principle is expanded. By utilizing the micro-nano processing technology, the spectrophotometric detection sensor can be made extremely small, and the whole size is as follows: the length is 30mm, and the width and the thickness are 20mm.
By utilizing the micro-nano manufacturing process technology which is mature at present, the chemical component detection micro-nano optical sensor based on the spectrum absorption principle can be manufactured in batches, the manufacturing cost is low, and the product consistency is good. The sensor does not need manual adjustment again by a user, and the refractive index and the curvature radius of the optical waveguide are considered at the beginning of design, so that the sensor can be molded at one time during manufacturing. And because the micro-nano manufacturing technology can integrate a large number of discrete elements on a substrate with a small area, each independent element required by the sensor, such as an optical waveguide and the like, can be integrated together, and all the elements can be manufactured at one time by using few manufacturing steps, therefore, the sensor is characterized by being capable of being prepared in a large scale at a low cost, needing no later manual adjustment and matching and being convenient to use. The sensor adopting different LED light sources can be used in parallel, and simultaneous detection of multiple places can be realized.
The spectrophotometric detection sensor provided by the invention has the advantages of low cost, small volume, convenience for large-scale laying and the like. By utilizing a micro-nano manufacturing technology, an optical component of the sensor is formed at one time, and an optical element and an optical structure are unified and integrated. The detection light channel and the reference light channel can be well constructed by processing the silicon substrate through silicon anisotropic wet etching. The construction of the micro-nano structure optical channel can greatly shorten the optical path measured by a spectrophotometry method, so that a detector can obtain a more excellent response value, and meanwhile, the construction of the reference optical channel and the signal comparison processing by the single-chip microcontroller can effectively eliminate errors caused by the self-attenuation of a light source. The spectrophotometric detection sensor provided by the invention integrates a mixer, a detection channel, an optical channel and the like required in spectrophotometric detection, so that the mixer, the detection channel, the optical channel and the like are integrated on a silicon substrate, the integration level of the sensor is improved, and the application field of the sensor is wider. Meanwhile, the spectrophotometric detection sensor fully applies two surfaces of the silicon substrate, the binding surface is used for mixing the solution and the reagent, the non-binding surface corrodes the optical channel, the optical channel is in the silicon substrate, and the optical loss is reduced while interference light is avoided. Meanwhile, SU-8 photoresist is added to the optical path part, and the optical waveguide is manufactured by utilizing the difference of refractive indexes of SiO2, air and SU-8, so that the total reflection of light inside the silicon substrate is ensured. And a part of the detection channel connected with the optical path is made into a lens by using SU-8 to ensure parallel light.
The spectrophotometric detection sensor provided by the invention promotes the development of the research field of the spectrophotometric detection sensor. On the premise of ensuring accurate detection, the sensor has longer service life, lower cost and higher practical application value.
Drawings
FIG. 1 is a perspective view of a spectrophotometric detection sensor according to the present invention;
FIG. 2 is a schematic bottom perspective view of a spectrophotometric detection sensor according to the present invention;
FIG. 3 is a perspective view of the spectrophotometric detecting sensor of the present invention in a separated state;
FIG. 4 is a schematic top view of a silicon substrate and an enlarged view of a slot corner of a detection channel;
FIG. 5 is a schematic bottom view of a silicon substrate with a single detection light source and an enlarged view of a portion of a light inlet slot;
FIG. 6 is a schematic bottom view of a silicon substrate using two detection light sources;
FIG. 7 is a schematic view showing changes in cross-sectional shapes of respective processes in a process of manufacturing a silicon substrate;
FIG. 8 is a schematic view of a partial section and a light path direction of a detection channel slot of the spectrophotometric detection sensor according to the present invention;
fig. 9 is a schematic view of water quality detection performed in a water environment by using the spectrophotometric detection sensor of the present invention.
Since the silicon substrate is thin compared with the glass substrate, the depth of the slotted structure on the silicon substrate and the width of the light-transmitting gap are both small and are in micron order, and the related drawings are schematic and do not correspond to actual proportions. Fig. 7 and 8 are schematic, and important features such as a light-transmitting slit having a small size are exaggerated and do not correspond to the actual sectional shape and scale.
The parts indicated by the reference numerals in the figures are: 1. a silicon substrate; 2. a glass substrate; 3. a detection channel slot; 4. a light inlet groove; 5. a light-emitting slot; 6. a first light-transmitting gap; 7. a second light-transmitting gap; 8. a light source slot; 9. a reference groove; 10. connecting grooves; 11. an optical waveguide; 12. a side wall; 13. a liquid interface to be tested; 14. an indicator interface; 15. injecting the liquid to be tested into the through hole; 16. an indicator injection through hole; 17. a merging tank; 18. a mixing channel; 19. a waste liquid tank; 20. waste liquid through holes; 21. and (4) a light-hydrophobic layer.
Detailed Description
The invention is described in further detail below with reference to the following examples of the drawings.
As shown in fig. 1 to 3, a spectrophotometric detection sensor includes a silicon substrate 1 and a glass substrate 2 which are bonded to each other, the glass substrate 2 covers the silicon substrate 1, and both the bonding surface and the bottom surface of the silicon substrate 1 are of a slotted structure formed by etching. As shown in fig. 2 or fig. 3, a detection channel groove 3 is formed in the bonding surface of the silicon substrate 1. As shown in fig. 1 or fig. 3, the glass substrate 2 is provided with: at least 1 liquid inlet channel that is used for to the liquid injection of detection channel groove 3 that communicates detection channel groove 3, at least 1 liquid outlet channel that is used for to outwards flowing back that communicates detection channel groove 3.
As shown in fig. 5 or fig. 6, the bottom surface of the silicon substrate 1 is provided with a light inlet groove 4 at a position corresponding to the starting side of the detection channel groove 3, and a light outlet groove 5 at a position corresponding to the final side of the detection channel groove 3. A first light-transmitting gap 6 penetrating through the silicon substrate 1 is formed between the starting side of the detection channel groove 3 and the light inlet groove 4 on the bottom surface of the silicon substrate 1; and a second light-transmitting gap 7 penetrating through the silicon substrate 1 is formed between the final side of the detection channel groove 3 and the light-emitting groove 5 on the bottom surface of the silicon substrate 1.
As shown in FIG. 4, a light source groove 8 and a reference groove 9 are formed beside a light inlet groove 4 on the bottom surface of a silicon substrate 1, a connection groove 10 is formed on the light inlet groove 4, and the light source groove 8 and the reference groove 9 are also respectively formed with a connection groove 10 and connected with the connection groove 10 of the light inlet groove 4.
The light source groove 8, the reference groove 9, each connecting groove 10, the light inlet groove 4, the first light transmitting gap 6 and the detection channel groove 3 start side to form a light source light channel cavity, the light outlet groove 5 and the second light transmitting gap 7 and the detection channel groove 3 end side to form a signal light channel cavity, the light source light channel cavity and the signal light channel cavity are filled with an optical waveguide 11 formed by liquid pouring and curing, and the optical waveguide 11 forms opposite side walls 12 on the start side and the end side of the detection channel groove 3 respectively. A detection light source, a reference light source and a photoelectric detector for photoelectric conversion are respectively arranged at the positions of the light source groove 8, the reference groove 9 and the light emergent groove 5 on the bottom surface of the silicon substrate 1.
As shown in FIG. 3, the side walls 12 of the light guide 11 on the initial side and the final side of the detection channel groove 3 on the bonding surface of the silicon substrate 1 are convex arc-shaped light-converging walls, and are formed into convex lens shapes.
As shown in fig. 3 or 4, a bonding surface of the silicon substrate 1 is respectively provided with a to-be-tested liquid interface 13 and an indicator interface 14, and the glass substrate 2 is respectively provided with a to-be-tested liquid injection through hole 15 and an indicator injection through hole 16 at positions corresponding to the to-be-tested liquid interface 13 and the indicator interface 14; a merging groove 17 is formed between the liquid interface 13 to be detected and the indicator interface 14, and a mixing channel 18 is formed between the merging groove 17 and the detection channel groove 3. The mixing channel 18 is in the shape of an S-shaped travel. As shown in fig. 3 or fig. 4, the glass substrate 2 is provided with 2 liquid outlet channels for discharging liquid to the outside, which are communicated with the detection channel groove 3, specifically: the binding surface of the silicon substrate 1 is respectively provided with 2 waste liquid pools 19 connected with the detection channel groove 3 at the two ends of the detection channel groove 3, and the glass substrate 2 is respectively provided with 2 waste liquid through holes 20 communicated with the outside at the corresponding positions of the 2 waste liquid pools 19.
As shown in fig. 5, the light source groove 8 and the reference groove 9 are symmetrically disposed at an upper side and a lower side of the light inlet groove 4, respectively, and the three and the connection groove 10 are arranged in a Y-shape. Alternatively, as shown in FIG. 6, 2 light source grooves 8 are symmetrically disposed obliquely above and below the light-entering groove 4, respectively, and the reference groove 9 is disposed outside the silicon substrate 1 in the horizontal direction along the connecting groove 10 of the light-entering groove 4. The latter needs to add a detection light source, but the detection effect is better.
By utilizing the micro-nano processing technology, the spectrophotometric detection sensor can be made extremely small, and the whole size is as follows: the length is 30mm, and the width and the thickness are 20mm. The silicon substrate 1 is a rectangular thin plate having the same size as the glass substrate 2, and the silicon substrate 1 is a thin plate having a thickness of 400 um to 450 um. The depth of the groove on the attaching surface of the silicon substrate 1 is about one half of the total thickness of the silicon substrate, and the depth of the groove on the bottom surface of the silicon substrate 1 is about one quarter of the total thickness of the silicon substrate. Thus, the remaining thickness of the silicon substrate 1 is also about one-fourth of its total thickness. That is, the depths of the first and second light-transmitting slits 6 and 7 are also about one fourth of the total thickness thereof. The residual thickness of the silicon substrate 1 is too thin, which naturally affects the physical strength of the silicon substrate 1, and if the residual thickness is too thick, the material is naturally wasted; therefore, the above arrangement is suitable. In addition, the inner cavity wall of the silicon substrate 1 after molding can be oxidized, and the formed silicon oxide layer is used as the light-sparse layer 21 of the internal optical waveguide 11, so that the optical transmission efficiency of the optical waveguide 11 is higher, and the detection effect is better.
The optical waveguide 11 is made of SU-8 polymer, the detection light source can be an LED light emitter or a xenon flash lamp with fixed wavelength, the reference light source can be an LED light emitter or a xenon flash lamp with fixed wavelength, and the photoelectric detector can be a photosensitive tube or a photodiode.
The invention discloses a manufacturing method of a spectrophotometry detection sensor, which comprises the steps of respectively manufacturing a silicon substrate 1 and a glass substrate 2, and then bonding the manufactured silicon substrate on the glass substrate 2; the method is characterized in that an MEMS processing technology is adopted for manufacturing the spectrophotometry detection sensor, and comprises the steps of oxidizing and photoetching a silicon substrate 1 to form a sample inlet and outlet channel, a mixing channel 18 and a detection channel, and then photoetching grooving, injecting photoresist, developing, exposing and curing are carried out on a non-binding surface of the silicon substrate 1 to form an optical component and an optical channel. The specific process for manufacturing the silicon substrate 1 is shown in fig. 7, and comprises the following steps:
step one, selecting a single-side polished silicon wafer with a (100) crystal face surface as a raw material of a silicon substrate 1; see fig. 7-1.
Secondly, carrying out oxidation treatment on two surfaces of the silicon substrate 1 to form a silicon oxide layer; see fig. 7-2.
Step three, spin-coating a photoresist layer on the binding surface of the silicon substrate 1 on which the silicon oxide layer is formed to form a photoresist layer; see fig. 7-3.
Developing and exposing the silicon substrate 1 coated with the photoresist, photoetching, and preparing a window for corrosion on the silicon oxide layer; see fig. 7-4.
Step five, etching the silicon oxide layer on the binding surface by using a corrosion liquid through a wet method to prepare a corrosion window; see fig. 7-5.
Spin-coating a photoresist layer on the binding surface of the silicon substrate 1 with the silicon oxide layer formed to form a photoresist layer; see fig. 7-6.
Step seven, developing and exposing the non-binding surface of the silicon substrate 1 coated with the photoresist, photoetching, and preparing a window for corrosion on the silicon oxide layer; see fig. 7-7.
Step eight, etching the silicon oxide layer on the non-binding surface of the silicon substrate 1 by using a corrosion liquid wet method to prepare a corrosion window; see fig. 7-8.
Step nine, removing all photoresist layers by using a mixed solution of H2SO4 and H2O 2; see fig. 7-9.
Step ten, corroding silicon without a silicon dioxide protection area by using a KOH solution, performing anisotropic wet etching on the 1 layer of the silicon substrate to prepare a required mixed channel 18 of a reagent and a sample, and controlling the depth of the channel by controlling the corrosion rate and the corrosion time to reach a preset depth value; see fig. 7-10.
Step eleven, carrying out oxidation treatment on the inner cavity wall of the silicon substrate 1 formed by wet etching, and taking the formed silicon oxide layer as the light-sparse layer 21 of the internal optical waveguide 11; see fig. 7-11.
Step twelve, pouring SU-8 polymer into the optical channel cavity of the silicon substrate 1, and leveling the polymer evenly to completely fill the optical channel cavity; see fig. 7-12.
And thirteen, developing and exposing the silicon substrate 1 filled with the SU-8 polymer to solidify and mold the SU-8 polymer, and preparing a side wall 12 which is in a convex arc shape and is positioned at the light inlet and outlet of the optical waveguide.
Fourteen, removing redundant unexposed SU-8 polymer by using a mixed solution of H2SO4 and H2O2, and cleaning the surface of the silicon substrate, the mixing channel and the detection channel by using ultrapure water.
The glass substrate 2 is manufactured by selecting glass with proper material and size, cutting the glass into glass sheets with the same size as the silicon substrate 1, and punching holes at positions corresponding to the silicon substrate 1, which are accessed to the sample port; as shown in fig. 1 and 3, a sample inlet and a sample outlet are formed on a glass substrate having the same size as the silicon substrate 1 at positions corresponding to the silicon substrate 1.
And then bonding the processed silicon substrate 1 and the glass sheet, aligning and bonding corresponding positions of a glass substrate layer and the main detection sensor silicon substrate 1 layer together to preliminarily form a detection sensor semi-finished product. In order to prevent the SU-8 polymer from falling off during bonding, the temperature needs to be controlled to 110 ℃ or lower. And after bonding is finished, adhering the required and proper LED light source, the required photosensitive tube and the like to corresponding positions, and leading out the required lead to obtain the complete spectrophotometric detection sensor. And the rear-end signal acquisition and processing circuit is accessed.
With the spectrophotometric detection sensor of the present invention, as shown in fig. 9, an electrochemical workstation and a computer are configured, and the detection sensor is connected with the electrochemical workstation and the computer to form a measurement system. Before measurement, the parameter measurement system is used for calibrating the linear corresponding relation between the current change of the spectrophotometric detection sensor and the amount (such as concentration) of a detection substance according to the Lambert beer law; after the linear corresponding relation between the current of a single detection sensor and the quantity of the substance is obtained through calibration, parameter detection is carried out, and the quantity of the substance to be detected is obtained through measuring the current change value of the detection sensor.
The trend of light when the spectrophotometric detection sensor of the invention is used for detection is explained as follows: fig. 8 is a schematic view of a partial section and a light path direction of a detection channel slot of the spectrophotometric detection sensor of the present invention, as shown in fig. 8, including a light inlet slot 4, a first light-transmitting slit 6, a detection channel slot 3, a second light-transmitting slit 7, and a light outlet slot 5, where arrows indicate light directions. The light inlet groove 4, the first light-transmitting gap 6, the second light-transmitting gap 7 and the light outlet groove 5 are all filled with optical waveguides 11. The light source light emitted by the detection light source reaches the light inlet groove 4 along the light source groove 8 and the reference light along the reference groove 9 through the connecting groove 10, the light source can be reflected due to the inclination of 54.7 degrees generated by the etching process, and then a beam of light parallel to and perpendicular to the liquid to be detected can be formed through the side wall 12 in the shape of a lens made of an optical waveguide. When light enters the detection channel groove 3 and is absorbed by the solution, signal light is generated, and the signal light is reflected by the side wall along the optical waveguide 11 to enter the light-emitting groove 5 and is finally received by the photoelectric detector attached to the light-emitting groove 5.
For example, the water quality detection is carried out by using the spectrophotometric detection core of the invention: the water quality detection method of the invention uses an electrochemical workstation, a computer and 1 spectrophotometric detection sensor, utilizes the good and stable linear relation between the photocurrent of the photosensitive tube and different illumination intensities, and the linear relation can be expressed as follows: i = XA + Y. From lambert beer's law and spectrophotometry, a = ∈ lc, and ∈ l are known, I = X (∈ lc) + Y. The X and Y values In the linear relation between the output current and the concentration of the spectrophotometric detection sensor are obtained by adjusting the concentration c of a detection object to be c1, c2, c3, \8230ccn, and measuring the currents I1, I2, I3, \8230incorresponding to the illumination intensity at one time by using an electrochemical workstation. The LED power supply and the photosensitive tube of the detection sensor are respectively connected with the electrochemical workstation and the computer through leads thereof. And (3) washing the spectrophotometric detection sensor by using a buffer solution, turning on a detection light source and a reference light source, and preheating for 1min. Three light sources are arranged to alternately emit light. And (3) introducing the sample into the detection sensor in a negative pressure sample introduction mode, and recording the current change of the detection sensor. Firstly, adding a sample into a detection sensor and recording the current change as a blank control; and then adding the sample and the indicator into the detection sensor, fully mixing the sample and the indicator in the mixing channel, detecting the sample after the sample and the indicator enter the flow cell, and recording the current value of the electrochemical workstation. The corresponding amount of the detection substance is calculated from the current value.
For example, the invention can be used for detecting the pH value of seawater: LED light sources with wavelengths of 434nm and 574nm are used as detection light sources, and an LED light source with a wavelength of 734nm is selected as a reference light source. Firstly, turning on a light source for preheating for 1min, and washing a channel in the detection sensor by using a seawater standard buffer solution to ensure that no other factors interfere in the channel; then, introducing a seawater sample to be detected into a detection sensor, and recording a current value as a blank control; then simultaneously adding a seawater sample and an acid-base indicator into the detection sensor, wherein the acid-base indicator is prepared in advance, dissolving high-purity m-cresol purple in a NaCl solution, the concentration of the m-cresol purple is 2mmol/L, and adjusting the pH value of the m-cresol purple solution to about 7.5 by adding NaOH and HCl; and recording current values of the electrochemical workstation at different wavelengths. And calculating by utilizing a secondary ionization equilibrium equation and the pH value through a rear-end processing circuit to obtain the pH value of the seawater.
For another example, the invention can be used for detecting the content of phosphorus in food: LED light sources with the wavelengths of 660nm and 440nm are adopted as detection light sources, and an LED light source with the wavelength of 750nm is selected as a reference light source. Firstly, food samples need to be pretreated, including washing, drying, crushing, extracting, separating, purifying and the like, a light source is turned on and preheated for 1min, and a channel inside a detection sensor is washed by standard stock solution and deionized water, so that no interference of other factors exists in the channel; then introducing the treated liquid to be detected into a detection sensor, and recording a current value as a blank contrast; then, simultaneously adding a solution to be detected and an ammonium molybdate solution into the detection sensor, keeping the mixed solution acidic, reacting phosphorus and ammonium molybdate under the acidic condition, and reducing the compound by hydroquinone and other substances to form molybdenum blue; subsequently, hydroquinone solution (2 g/L) was added; and after standing, recording current values of the electrochemical workstation at different wavelengths. At the 660nm wave band, the light absorption value of the solution is in direct proportion to the content of the phosphorus element, and the content of the phosphorus element in the solution to be detected is calculated according to the Lambert beer law.
For another example, the method can be used for detecting the content of nitrite in the water for cultivation: LED light sources with the wavelengths of 474nm and 530nm are adopted as detection light sources, and an LED light source with the wavelength of 750nm is selected as a reference light source. Preheating for 1min with light source turned on, and using NaNO 2 The standard solution washes a channel in the detection sensor to ensure that no other factors interfere in the channel; then introducing a water sample for cultivation to be detected and sulfanilic acid solution (4 g/L) into a detection sensor, and recording a current value as a blank control; then adding a pure solution of diethylaniline into the detection sensor, wherein the reaction input is carried out in a low-temperature environment; and after standing, recording current values of the electrochemical workstation at different wavelengths. And calculating the content of nitrite in the aquaculture water according to the Lambert beer law.
Claims (10)
1. The utility model provides a spectrophotometry detection sensor, includes silicon chip (1) and glass substrate (2) of interbonding, glass substrate (2) cover silicon chip (1) is higher authority, and the binding face and the bottom surface of silicon chip (1) are the fluting structure that forms through the etching process, and its characterized in that sets up detection channel groove (3) at silicon chip (1) binding face, and glass substrate (2) have been seted up: at least 1 liquid inlet channel which is communicated with the detection channel groove (3) and used for injecting liquid into the detection channel groove (3), and at least 1 liquid outlet channel which is communicated with the detection channel groove (3) and used for discharging liquid outwards; a light inlet groove (4) is formed in the bottom surface of the silicon substrate (1) at a position corresponding to the starting side of the detection channel groove (3), and a light outlet groove (5) is formed in the position corresponding to the final side of the detection channel groove (3); a first light-transmitting gap (6) penetrating through the silicon substrate (1) is formed between the starting side of the detection channel groove (3) and the light inlet groove (4) in the bottom surface of the silicon substrate (1); a second light-transmitting gap (7) penetrating through the silicon substrate (1) is formed between the final side of the detection channel groove (3) and the light-emitting groove (5) on the bottom surface of the silicon substrate (1); a light source groove (8) and a reference groove (9) are formed beside the light inlet groove (4) on the bottom surface of the silicon substrate (1), the light inlet groove (4) is provided with a connecting groove (10), and the light source groove (8) and the reference groove (9) are also respectively provided with the connecting groove (10) and are connected with the connecting groove (10) of the light inlet groove (4); the light source groove (8), the reference groove (9), each connecting groove (10), the light inlet groove (4) and the first light transmitting gap (6) form a light source light channel cavity till the starting side of the detection channel groove (3), the light outlet groove (5) and the second light transmitting gap (7) form a signal light channel cavity till the ending side of the detection channel groove (3), the light source light channel cavity and the signal light channel cavity are filled with an optical waveguide (11) which is formed by liquid pouring and then curing, and the optical waveguide (11) respectively forms opposite side walls (12) at the starting side and the ending side of the detection channel groove (3); and a detection light source, a reference light source and a photoelectric detector for photoelectric conversion are respectively arranged at the positions of the light source groove (8), the reference groove (9) and the light-emitting groove (5) on the bottom surface of the silicon substrate (1).
2. The spectrophotometric detecting sensor according to claim 1, wherein the side walls (12) of the light guide (11) on the initial side and the final side of the detecting channel groove (3) on the abutting surface of the silicon substrate (1) are light-gathering walls in the shape of a convex circular arc to form convex lenses.
3. The spectrophotometric detecting sensor according to claim 1, wherein the bonding surface of the silicon substrate (1) is provided with a liquid interface (13) to be detected and an indicator interface (14), respectively, and the glass substrate (2) is provided with a liquid injection through hole (15) to be detected and an indicator injection through hole (16) at positions corresponding to the liquid interface (13) to be detected and the indicator interface (14), respectively; a junction groove (17) is formed between the liquid interface (13) to be detected and the indicator interface (14), and a mixing channel (18) is formed between the junction groove (17) and the detection channel groove (3).
4. The spectrophotometric detecting sensor of claim 3 wherein said mixing channel (18) is in the shape of an S-shaped travel.
5. The spectrophotometric detecting sensor according to claim 1, wherein the glass substrate (2) is provided with 2 liquid outlet channels for discharging liquid to the outside, which are communicated with the detecting channel groove (3), specifically: the silicon substrate (1) binding face sets up 2 waste liquid ponds (19) of connecting detection channel groove (3) respectively by its detection channel groove (3) both ends, glass substrate (2) are seted up 2 and are communicated with each other waste liquid through-hole (20) with the external world respectively in 2 waste liquid ponds (19) correspondence punishment.
6. The spectrophotometric detecting sensor of claim 1, wherein the light source groove (8) and the reference groove (9) are symmetrically disposed at an upper oblique side and a lower oblique side of the light inlet groove (4), respectively, and the three and the connecting groove (10) thereof are arranged in a Y shape.
7. The spectrophotometric detecting sensor according to claim 1, wherein the number of the light source grooves (8) is 2, and the reference grooves (9) are disposed on the outer side of the silicon substrate (1) in the horizontal direction along the connecting grooves (10) of the light inlet grooves (4), and are disposed symmetrically above and below the light inlet grooves (4), respectively.
8. The spectrophotometric detecting sensor according to claim 1, wherein the silicon substrate (1) and the glass substrate (2) are rectangular thin blocks with the same size, the silicon substrate (1) is a thin block with a thickness of 400 um to 450 um, the depth of the groove on the abutting surface of the silicon substrate (1) is half of the total thickness of the silicon substrate, the depth of the groove on the bottom surface of the silicon substrate (1) is a quarter of the total thickness of the silicon substrate, and the depths of the first light-transmitting slit (6) and the second light-transmitting slit (7) are also a quarter of the total thickness of the silicon substrate.
9. The spectrophotometric detecting sensor according to claim 1, wherein the inner cavity wall of the molded silicon substrate (1) is oxidized to form a silicon oxide layer as the optically sparse layer (21) of the internal optical waveguide (11).
10. The spectrophotometric detecting sensor of any one of claims 1 to 9, wherein the optical waveguide (11) is made of SU-8 polymer, the detecting light source is selected from a fixed wavelength LED illuminator or a flashing xenon lamp bare lamp, the reference light source is also selected from a fixed wavelength LED illuminator or a flashing xenon lamp bare lamp, and the photodetector is selected from a photosensitive tube or a photodiode.
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