CN111257288A - Concentration detection sensor, detection method thereof, and concentration detection device - Google Patents
Concentration detection sensor, detection method thereof, and concentration detection device Download PDFInfo
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- CN111257288A CN111257288A CN202010238359.8A CN202010238359A CN111257288A CN 111257288 A CN111257288 A CN 111257288A CN 202010238359 A CN202010238359 A CN 202010238359A CN 111257288 A CN111257288 A CN 111257288A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/21—Polarisation-affecting properties
Abstract
The invention provides a concentration detection sensor, a detection method thereof and a concentration detection device, wherein the concentration detection sensor comprises a substrate, a dielectric layer arranged on the substrate and a waveguide layer arranged on the dielectric layer, the waveguide layer comprises a waveguide film layer, an anisotropic nano-pillar array layer formed on the waveguide film layer and a modifying enzyme formed on the nano-pillar array layer, and the modifying enzyme is used for adsorbing a substance to be detected so as to change the effective reflectivity of the concentration detection sensor and further detect the concentration of the substance to be detected.
Description
Technical Field
The invention relates to the field of concentration detection, in particular to a concentration detection sensor, a detection method thereof and a concentration detection device.
Background
Conventional surface plasmon resonance sensors generally comprise a three-layer structure: a base layer, a metal layer, and a cover layer. A laser irradiates the surface plasma resonance sensor according to different incidence angles, light is coupled into the sensor at a specific angle, and the reflected light intensity changes accordingly. The coupling angle depends on the effective reflectivity of the surface plasmon resonance sensor, and is mainly affected by the reflectivity of the covering layer (solution to be measured) when the substrate layer and the metal layer are fixed. The information about the cover layer is analyzed by analyzing the change in the coupling angle. However, the penetration depth of the conventional surface plasmon resonance sensor is only about 100nm, and the conventional surface plasmon resonance sensor is mainly used for analyzing substances of molecular size grades, such as heavy metal ions, glucose, proteins and the like.
The optical waveguide sensor is similar to the surface plasmon resonance sensor and includes a four-layer structure of a base layer, a metal layer, a waveguide layer, and a cover layer. Compared with the surface plasma resonance sensor, the optical waveguide sensor adds the waveguide layer with the thickness of hundreds of nanometers between the metal layer and the covering layer, not only provides a plurality of waveguide propagation modes, but also greatly increases the penetration depth of the waveguide. The optical waveguide sensor is not only applied to the detection of small molecules, but also has important application in the detection of micron-scale organisms such as bacteria, cells and the like. Optical waveguide sensors have become an important part of optical sensors with ultra-high sensitivity in complex micro-scale detection.
The sensitivity and detection modality of the optical waveguide sensor depend mainly on the design of the waveguide layer. The common waveguide layer materials at present include porous anodic aluminum oxide films, porous titanium dioxide films, hydrogel films, array films made of different materials filled with anodic aluminum oxide as a template, and the like. The waveguide layer is not subjected to special structure treatment, and modified enzyme is easy to have the defect of low efficiency of specific adsorption of polar molecules due to low enzyme adhesion.
Disclosure of Invention
The technical problem to be solved by the embodiments of the present invention is to provide a concentration detection sensor, a detection method thereof, and a concentration detection device, which have high sensitivity.
In order to solve the above technical problem, an embodiment of the present invention provides a concentration detection sensor, including a substrate, a metal layer disposed on the substrate, and a waveguide layer disposed on the metal layer, where the waveguide layer includes a dielectric layer, an anisotropic nanopillar array layer formed on the dielectric layer, and a modifying enzyme formed on the nanopillar array layer, and the modifying enzyme is used to adsorb a substance to be detected, so as to change an effective reflectivity of the concentration detection sensor, and further detect a concentration of the substance to be detected.
Optionally, a cladding layer disposed over the waveguide layer is also included.
Optionally, the substrate is a prismatic structure.
Optionally, the nanopillar array layer is made of a silicon dioxide material.
The embodiment of the present invention further provides a concentration detection apparatus, which includes a light source, a photodetector and the concentration detection sensor of any one of claims 1 to 4 disposed between the light source and the photodetector, wherein the light emitted from the light source is reflected by the concentration detection sensor and received by the photodetector.
Optionally, the concentration detecting device further comprises a polarizer disposed between the light source and the concentration detecting sensor, and light emitted from the light source passes through the polarizer and is incident into the concentration detecting sensor.
Optionally, the concentration detection device further comprises a non-polarization beam splitter prism arranged between the polarizer and the concentration detection sensor, and the non-polarization beam splitter prism reflects the light emitted by the polarizer and enters the concentration detection sensor.
Optionally, the concentration detection device further comprises a first reflecting mirror disposed between the non-polarization beam splitter prism and the concentration detection sensor, and the first reflecting mirror reflects light emitted by the non-polarization beam splitter prism to form incident light which perpendicularly enters the concentration detection sensor.
Optionally, the concentration detection device further comprises a polarization analyzer located between the concentration detection sensor and the photodetector, and light reflected by the concentration detection sensor passes through the polarization analyzer and enters the photodetector.
Optionally, the concentration detection device further comprises a second reflecting mirror disposed between the concentration detection sensor and the analyzer, and the second reflecting mirror emits the light reflected by the concentration detection sensor into the analyzer.
The embodiment of the present invention further provides a detection method of the foregoing concentration detection sensor, including:
establishing a reflectivity mapping table containing solutions of substances to be detected with different concentrations;
placing a concentration detection sensor in a solution to be detected;
measuring the reflectivity of the solution to be detected through the concentration detection sensor;
and comparing the reflectivity of the solution to be detected with the reflectivity mapping table to determine the concentration of the substance to be detected in the solution to be detected.
The embodiment of the invention provides a concentration detection sensor, a detection method thereof and a concentration detection device, wherein the concentration detection sensor selectively adsorbs polar molecules to be detected by forming a modification enzyme on a nano-column array layer so as to change the reflectivity of the concentration detection sensor, and the concentration of the polar molecules to be detected is determined by the reflectivity, so that the concentration of the polar molecules to be detected is detected by an optical waveguide method.
The concentration detection sensor provided by the embodiment of the invention is provided with the anisotropic nano-column array layer, so that the specific surface area of the nano-column array layer is increased, the attachment efficiency of the modification enzyme is increased, and the efficiency of adsorbing molecules is improved.
Of course, not all of the advantages described above need to be achieved at the same time in the practice of any one product or method of the invention. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the embodiments of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the example serve to explain the principles of the invention and not to limit the invention. The shapes and sizes of the various elements in the drawings are not to scale and are merely intended to illustrate the invention.
FIG. 1 is a schematic structural view of a concentration detection sensor according to a first embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a concentration sensor according to a first embodiment of the present invention;
FIG. 3 is a multilayer film reflection model of the concentration sensor according to the first embodiment of the present invention;
FIG. 4 is a reflectance angle spectrum of the concentration detecting sensor according to the first embodiment of the present invention;
FIG. 5 is a schematic structural diagram of a concentration detecting device according to a second embodiment of the present invention;
FIG. 6 is a diagram illustrating the reflectivity of a sensor and the mass fraction of a substance according to a third embodiment of the present invention.
Detailed Description
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
Unless otherwise defined, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this disclosure belongs. The use of "first," "second," and similar terms in this disclosure is not intended to indicate any order, quantity, or importance, but rather is used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items. "upper", "lower", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
In the research, the inventors of the present application found that: the existing optical waveguide sensor only has a simple dielectric layer, such as a silicon dioxide film, and the dielectric layer is not subjected to special structural treatment, so that the defect of low efficiency of polar molecule adsorption exists, and the sensitivity is low.
In order to solve the problems of low sensitivity and the like of the conventional optical waveguide sensor, an embodiment of the present invention provides a concentration detection sensor, which includes a substrate, a metal layer disposed on the substrate, and a waveguide layer disposed on the metal layer, where the waveguide layer includes a dielectric layer, an anisotropic nanopillar array layer formed on the dielectric layer, and a modifying enzyme formed on the nanopillar array layer, and the modifying enzyme is used to adsorb a substance to be detected, so as to change the effective reflectivity of the concentration detection sensor, and further detect the concentration of the substance to be detected.
The technical solution of the present invention will be described in detail by the following specific examples.
First embodiment
Fig. 1 is a schematic structural view of a concentration detection sensor according to a first embodiment of the present invention. As shown in fig. 1, an embodiment of the present invention provides a concentration detection sensor, including a substrate 100, a metal layer 200 disposed on the substrate 100, and a waveguide layer 300 disposed on the metal layer 200, where the waveguide layer 300 includes a dielectric layer 310, an anisotropic nanopillar array layer 320 formed on the dielectric layer 310, and a modifying enzyme 330 formed on the nanopillar array layer 320, and the modifying enzyme 330 is used for adsorbing a substance to be detected to change an effective reflectivity of the concentration detection sensor. The substrate 100 is a prism structure, and the reflectivity of the substrate 100 is 1.517. The metal layer 200 had a film thickness of 45nm and a reflectance of 0.15+ 3.2. The nano-pillar array layer 320 is made of silicon dioxide, the effective reflectivity of the nano-pillar array layer is about 1.396, the film thickness is 400nm, and the pillar height of the nano-pillar array layer 320 is 100 nm.
Fig. 2 is a schematic structural diagram of a concentration detection sensor according to a first embodiment of the present invention. As shown in fig. 2, the concentration detection sensor of the embodiment of the present invention further includes a covering layer 400 disposed on the waveguide layer 300. The cover layer 400 is a solution to be measured, for example, the cover layer 400 is deionized water, the reflectance is 1.33, the wavelength of incident light of the cover layer 400 is 632.8nm, and the total reflection angle θ is asin (1.33/1.517) is 61.25 °, so that the incident angle of the cover layer 400 is varied within a range of 60 to 70 degrees, and the variation precision is 0.01 °.
The embodiment of the invention selectively adsorbs polar molecules by the modified enzyme 330, thereby achieving the technical effect of measuring the concentration of the solution to be measured in real time on line and with high sensitivity.
The concentration detection sensor provided by the embodiment of the invention can be applied to biomolecule detection. For example, the concentration detection sensor of the embodiment of the invention can be used for measuring the concentration of blood glucose in blood, so as to solve the technical problems that more blood needs to be extracted and the detection time is long in blood glucose measurement.
In the embodiment of the invention, the nano-column array layer 320 has polarity, can adsorb most polar molecules, such as glucose, protein and the like, and is used for adsorbing a certain specific polar molecule through the modifying enzyme 330, so that the concentration of the solution to be tested is obtained on the basis of lower concentration of the test sample solution, and the nano-column array layer has higher sensitivity.
The principle of detecting the concentration of the solution to be detected by the concentration detection sensor in the embodiment of the invention is as follows:
fig. 3 is a multilayer film reflection model of the concentration detection sensor according to the first embodiment of the present invention. As shown in FIG. 3, with respect to the concentration detection sensor of the present embodiment, n1Layer film, n2Layer film, n3Layer film and n4The layer film is reflected, and a multilayer film reflection model in the concentration detection sensor of the embodiment is established. Wherein n is the concentration of the substance in the sensor1Film as a substrate, n2The film is a metal layer, n3The layer being a waveguide layer, n4The film being a cover layer, d1Is the thickness of the substrate, d2Is the thickness of the metal layer, d3Thickness of the waveguide layer, d4Is the thickness of the cover layer.
The light is incident from the substrate, reflected by the metal layer, the waveguide layer and the covering layer in sequence, and reflected from the substrate. R1234Reflectivity, R, of four layers of film for substrate, metal layer, waveguide layer and cover layer1234Comprises the following steps:
R123reflectivity of three layers of film for substrate, metal layer and waveguide layer, R123Comprises the following steps:
rijis the reflectance coefficient between media i and j, rijComprises the following steps:
wherein k isz,iIs the wave vector in z direction in medium i, niIn the present invention, the reflectance of the medium i is represented by ρ, TE polarization is represented by ρ 0, and TM polarization is represented by ρ 1.λ is the incident wavelength, N is the x-direction wave vector normalized tangent part, and θ i is the incident angle into the medium i. From fresnel's law, it is known that N is equal in value in each layer of the medium.
Wherein N is:
in the embodiment of the invention, the nano-pillar array layers are not uniformly distributed and are not arranged orderly, so that the effective reflectivity is calculated by a general formula. According to the Bruggeman combined approximate Fresnel formula, when the modification enzyme on the surface of the nano-pillar array layer adsorbs specific polar molecules, for example, the modification enzyme adsorbs glucose molecules, the effective reflectivity calculation formula of the nano-pillar array layer is as follows:
wherein f is1、f2And f3The volume fraction of analytical molecules, n, of the nanocolumn array layer, the specific polar molecule and the modified enzyme adsorbed with the specific polar molecule, respectively, in the three-phase mixture1，n2，n3And n is the reflectivity of the nano-column array layer, the specific polar molecule and the modified enzyme which adsorbs the specific polar molecule and the effective reflectivity after three-phase mixing respectively.
According to the theoretical formula, when the concentration detection sensor tests the solution to be tested, the incident angle of the incident light of the concentration detection sensor is continuously changed to obtain an incident angle-reflectivity curve, and a resonance groove is formed on the incident angle-reflectivity curve. The angle corresponding to the lowest point of the resonance groove is the resonance angle. The resonance angle depends on the effective reflectivity of the waveguide structure. When the concentration of the solution layer (covering layer) to be measured changes, namely the reflectivity of the solution to be measured changes, the resonance angle is deviated. Because the resonance groove on the incident angle-reflectivity curve has very narrow full width at half maximum, namely the slope of the reflectivity near the resonance groove along with the change of the angle is very large, the change of the reflectivity can be detected by fixing the incident angle to the vicinity of the resonance angle, so that the small change of the effective reflectivity of the waveguide layer can be detected, and the change of the concentration of the solution to be detected can be analyzed.
Fig. 4 is a reflectance angle spectrum of the concentration detection sensor according to the first embodiment of the present invention. The method for obtaining the incident angle-reflectivity curve of the concentration detection sensor in the embodiment of the invention is explained by taking test deionized water as an example. The method for obtaining the incident angle-reflectivity curve by the concentration detection sensor comprises the following steps: deionized water is introduced into a flow channel of the concentration detection sensor for a period of time, so that the whole system reaches a stable state; then, under the condition that the entire flow channel of the concentration detection sensor is filled with deionized water, the incident angle is continuously adjusted, the corresponding reflectivity is measured, and an incident angle-reflectivity curve of the deionized water is drawn, as shown in fig. 4.
The incident angle-reflectivity curves of different waveguide layers can be drawn according to the above method, for example, when the reflectivity of the waveguide layer varies from 1.36 to 1.42, the corresponding incident angle varies.
Second embodiment
Fig. 5 is a schematic structural diagram of a concentration detection apparatus according to a second embodiment of the present invention. As shown in fig. 4, based on the technical idea of the foregoing embodiment, an embodiment of the present invention further provides a concentration detecting apparatus, which includes a light source 10, a photodetector 20, and a concentration detecting sensor 30 disposed between the light source 10 and the photodetector 20, wherein light emitted from the light source 10 is reflected by the concentration detecting sensor 30 and received by the photodetector 20. The intensity of the reflected light is measured by the photodetector 20 to measure the reflectance of the concentration detection sensor 30, thereby determining the concentration of the solution to be detected.
As shown in fig. 5, the concentration detecting apparatus according to the embodiment of the present invention further includes a polarizer 40 disposed between the light source 10 and the concentration detecting sensor 30, and the light emitted from the light source 10 passes through the polarizer 40 and enters the concentration detecting sensor 30. The polarizer 40 includes a first polarizer, a second polarizer, and a quarter-wave plate disposed between the first polarizer and the second polarizer.
As shown in fig. 5, the concentration detection apparatus according to the embodiment of the present invention further includes a non-polarization beam splitter prism 50 disposed between the polarizer 40 and the concentration detection sensor 30, and the non-polarization beam splitter prism 50 reflects the light emitted from the polarizer 40 and enters the concentration detection sensor 30.
As shown in fig. 5, the concentration detecting apparatus according to the embodiment of the present invention further includes a first reflecting mirror 60 disposed between the non-polarizing beam splitter prism 50 and the concentration detecting sensor 30, and the first reflecting mirror 60 reflects the light emitted from the non-polarizing beam splitter prism 50 to form an incident light vertically entering the concentration detecting sensor 30.
As shown in fig. 5, the concentration detecting apparatus according to the embodiment of the present invention further includes an analyzer 70 located between the concentration detecting sensor 30 and the photodetector 20, and the light reflected by the concentration detecting sensor 30 passes through the analyzer 70 and enters the photodetector 20.
As shown in fig. 5, the concentration detecting apparatus according to the embodiment of the present invention further includes a second reflecting mirror 80 disposed between the concentration detecting sensor 30 and the analyzer 70, and the second reflecting mirror 80 emits the light reflected by the concentration detecting sensor 30 into the analyzer 70.
As shown in fig. 5, the concentration detecting apparatus according to the embodiment of the present invention further includes a third reflecting mirror 90 and a fourth reflecting mirror 100 respectively disposed above the non-polarizing beam splitter prism 50, where the third reflecting mirror 90 and the fourth reflecting mirror 100 are used for reflecting the light reflected by the non-polarizing beam splitter prism 50 to enter the photodetector 20 to obtain the reference light intensity (I)reference)。
Third embodiment
Based on the technical idea of the foregoing embodiment, an embodiment of the present invention further provides a detection method of a concentration detection sensor, including:
s1, establishing a reflectivity mapping table containing the solutions of the substances to be detected with different concentrations;
s2, placing the concentration detection sensor in a solution to be detected;
s3, measuring the reflectivity of the solution to be detected through the concentration detection sensor;
s4, comparing the reflectivity of the solution to be detected with the reflectivity mapping table, and determining the concentration of the substance to be detected in the solution to be detected.
Fig. 6 is a schematic diagram of the reflectivity of the concentration detection sensor and the mass fraction of the substance to be detected according to the embodiment of the invention. Specifically, step S3 includes:
(1) firstly, deionized pure water is introduced for measurement IglassAnd (3) changing the polarization state of the incident light to obtain the incident polarization direction and the polarization angle with the highest reflectivity, such as 63 degrees, and measuring the subsequent measurement according to the polarization state and the incident angle.
(2) And measuring a reflectivity mapping table fitted with reflection angles of solutions mixed with glucose with different concentrations for later-stage actual measurement of unknown concentration samples, respectively mixing 1g/L to 6g/L of glucose in deionized water, and measuring the change condition of the reflectivity, as shown in FIG. 6.
(3) The incident angle is changed to be measured in the range of 60-70 degrees, and the ratio R-I is obtainedreal/Iglass，Ireal＝Isignal/Ireference. Wherein, IsignalTo test the intensity of the reflected light obtained, IreferenceFor reference light intensity, IrealFor measuring the ratio of the reflected intensity to the reference intensity, IglassIs the value of the intensity of the reflected light from the substrate. According to the formula, the reflection angle with the ratio R higher than 0.6 can be obtained, and the corresponding reflectivity is fitted and calculated, wherein the reflectivity is the reflectivity of the solution to be detected.
By calculating the quality parameter FOM ═ Δ θ/(Δ nX τ), it can be obtained that the detection method of the concentration detection sensor of the embodiment of the present invention has high sensitivity. Wherein, delta theta is the reflection angle change quantity, delta n is the reflectivity change quantity, and tau is the half-height width of the reflectivity angle spectrum, the measurement quality parameters are obtained, the linearity of the concentration change and the measured value is evaluated, and the measurement sensitivity is obtained. That is, when the reflectance is changed by a certain value, a finer reflectance change can be characterized when the deviation of the reflection angle is larger, so that higher concentration change accuracy can be measured.
Although the embodiments of the present invention have been described above, the above description is only for the convenience of understanding the present invention, and is not intended to limit the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (11)
1. The concentration detection sensor is characterized by comprising a substrate, a metal layer arranged on the substrate and a waveguide layer arranged on the metal layer, wherein the waveguide layer comprises a medium layer, an anisotropic nano-pillar array layer formed on the medium layer and a modifying enzyme formed on the nano-pillar array layer, and the modifying enzyme is used for adsorbing a substance to be detected so as to change the reflectivity of the concentration detection sensor and further detect the concentration of the substance to be detected.
2. The concentration detection sensor according to claim 1, further comprising a cover layer disposed over the waveguide layer.
3. The concentration detection sensor according to claim 1, wherein the substrate is a prism structure.
4. The concentration detection sensor according to claim 1, wherein the nanopillar array layer is made of silicon dioxide.
5. A concentration detecting apparatus, comprising a light source, a photodetector and the concentration detecting sensor of any one of claims 1 to 4 disposed between the light source and the photodetector, wherein the light emitted from the light source is reflected by the concentration detecting sensor and received by the photodetector.
6. The concentration detection apparatus according to claim 5, further comprising a polarizer disposed between the light source and the concentration detection sensor, wherein the light emitted from the light source passes through the polarizer and enters the concentration detection sensor.
7. The concentration detection apparatus according to claim 6, further comprising a non-polarizing beam splitter prism disposed between the polarizer and the concentration detection sensor, wherein the non-polarizing beam splitter prism reflects the light emitted from the polarizer and enters the concentration detection sensor.
8. The concentration detection apparatus according to claim 7, further comprising a first reflecting mirror disposed between the non-polarizing beam splitter prism and the concentration detection sensor, wherein the first reflecting mirror reflects the light emitted from the non-polarizing beam splitter prism to form an incident light that enters the concentration detection sensor perpendicularly.
9. The apparatus according to claim 5, further comprising an analyzer located between the concentration sensor and the photodetector, wherein the light reflected by the concentration sensor passes through the analyzer and enters the photodetector.
10. The apparatus according to claim 9, further comprising a second reflecting mirror disposed between the concentration sensor and the analyzer, the second reflecting mirror emitting the light reflected by the concentration sensor into the analyzer.
11. A method of detecting the concentration detection sensor according to any one of claims 1 to 4, comprising:
establishing a reflectivity mapping table containing solutions of substances to be detected with different concentrations;
placing a concentration detection sensor in a solution to be detected;
measuring the reflectivity of the solution to be detected through the concentration detection sensor;
and comparing the reflectivity of the solution to be detected with the reflectivity mapping table to determine the concentration of the substance to be detected in the solution to be detected.
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