CN119394921A - A metasurface for humidity detection, preparation method thereof and humidity sensor - Google Patents
A metasurface for humidity detection, preparation method thereof and humidity sensor Download PDFInfo
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- CN119394921A CN119394921A CN202510000856.7A CN202510000856A CN119394921A CN 119394921 A CN119394921 A CN 119394921A CN 202510000856 A CN202510000856 A CN 202510000856A CN 119394921 A CN119394921 A CN 119394921A
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Abstract
本发明提供一种用于湿度检测的超构表面、其制备方法以及湿度传感器，涉及光学器件领域，本发明提供的用于湿度检测的超构表面，包括层叠设置的传感层、透明氧化铝层和金镜，传感层包括对照模组和检测模组，所述对照模组和所述检测模组的排布在光学能带上呈现对称保护的连续域中束缚态，所述金镜包括自上而下层叠设置的金层和钛层。本发明提供的超构表面所支持的对称保护的连续域中束缚态有强大的光学增强效应其保证了其能够实现宽带高灵敏度湿度测量，其使用较小的结构尺寸即保证了其具有远小于电学传感器的响应速度以及复原能力，具有结构简单、尺寸小、测量范围宽、灵敏度高、响应速度快、环境适应性强、稳定性高的优点，具有广阔的应用前景。
The present invention provides a metasurface for humidity detection, a preparation method thereof and a humidity sensor, and relates to the field of optical devices. The metasurface for humidity detection provided by the present invention comprises a sensing layer, a transparent aluminum oxide layer and a gold mirror arranged in a stacked manner, the sensing layer comprises a reference module and a detection module, the arrangement of the reference module and the detection module presents a bound state in a continuous domain with symmetrical protection on an optical energy band, and the gold mirror comprises a gold layer and a titanium layer stacked from top to bottom. The bound state in the continuous domain with symmetrical protection supported by the metasurface provided by the present invention has a strong optical enhancement effect, which ensures that it can achieve broadband high-sensitivity humidity measurement, and the use of a smaller structural size ensures that it has a response speed and recovery ability far less than that of an electrical sensor, and has the advantages of simple structure, small size, wide measurement range, high sensitivity, fast response speed, strong environmental adaptability and high stability, and has broad application prospects.
Description
Technical Field
The invention relates to the field of optical devices, in particular to a super-structured surface for humidity detection, a preparation method thereof and a humidity sensor.
Background
Currently, humidity sensors mainly adopt an electrical humidity sensor which relies on measuring the physical property change of a humidity sensitive material under different environmental humidities, the electrical humidity sensor is widely applied because the electrical humidity sensor has a relatively simple structure, the sensor mainly reflects the environmental humidities through the relative electrical property change of the humidity sensitive material under different environmental humidities when measuring the environmental humidities, the sensing range of the electrical humidity sensor is generally narrow and concentrated in a high humidity range due to the fact that the electrical property of the humidity sensitive material is not obvious under low humidities, moreover, the electrical humidity sensor needs to monitor the electrical property change of the humidity sensitive material through an electrode, the aging of the electrode exposed to the external environment in the air can lead to the reduction of the sensor precision, and in addition, the electrical humidity sensor is difficult to be applied to the extreme environments of erodible metal electrodes such as acid, alkali and the like. Although the conventional optical humidity sensor can avoid the problem of aging of the metal electrode, the humidity sensing of the humidity sensitive material is difficult to realize in a high-sensitivity and broadband sensing range because the change of the optical parameters of the humidity sensitive material is tiny under different humidities.
Disclosure of Invention
The invention aims to solve the technical problem of improving the environmental adaptability of the humidity sensor and the sensitivity of broadband humidity sensing.
In order to solve the above problems, a first aspect of the present invention provides a super-structured surface for humidity detection, where the super-structured surface includes a sensing layer, a transparent alumina layer and a gold mirror that are stacked, the sensing layer includes a control module and a detection module, the control module and the detection module are arranged in a continuous domain binding state that is symmetrically protected on an optical energy band, and the gold mirror includes a gold layer and a titanium layer that are stacked from top to bottom.
Preferably, the material of the detection module is a high molecular polymer or ceramic. In the technical scheme provided by the invention, the detection module is made of a material which is sensitive to humidity and can reversibly change the form spectrum after reacting with water.
Preferably, the form of the detection module is selected from any one of a grating structure, a waveguide structure and a grating-waveguide composite structure.
Preferably, the control module is any one of glass, ceramic and high molecular polymer. In the technical scheme provided by the invention, the material of the detection module is a material which is insensitive to humidity and has unchanged morphological spectrum after the detection module reacts with water.
Preferably, the form of the control module is selected from any one of a grating structure, a square array and a disk array.
Preferably, the thickness range of the transparent alumina layer is 100nm or less, the thickness of the gold layer is 100nm or more, and the thickness range of the titanium layer is 3-10 nm. In the technical scheme provided by the invention, the transparent aluminum oxide layer has the function of enhancing the amplifying sensing function, and the gold layer has the function of being used as a reflecting layer to ensure that light energy is fully reflected.
In the super-structured surface for humidity detection, the shape and spectrum of the control module cannot change along with humidity change, and the shape of the detection module can reversibly change along with humidity change. The arrangement of the control module and the detection module presents a domain-wide bound state of symmetric protection on the optical band, based on which the control module and the detection module can change the symmetry of the control module-detection module by sensing the change of the external humidity. On this basis, when humidity changes, the refractive index of the detection module changes due to the morphological change of the detection module, which breaks the symmetry of the control module-detection module in both dielectric constant and geometry directions. At this time, the continuous confinement state at the point of the energy band Γ supported by the symmetrical structure is converted into a quasi-continuous domain confinement state in the asymmetrical structure, so that a mode corresponding to a wavelength appears on the spectrum. Along with the change of the external humidity, the asymmetry of the system is different, so that the degree of the continuous bound state in the structure is changed into the bound state in the quasi-continuous domain, and the bound state in the quasi-continuous domain shows different quality factors (Q factors) under different external humidities. In addition, high quality factor modes experience greater losses in the structure due to gold metal losses, resulting in lower relative intensities of the modes. In addition, due to the structural change, certain chromatic dispersion is generated in the process of the transition of the constraint state in the quasi-continuous domain, so that the external humidity can be defined by the mode Q factor, the mode spectrum displacement and the mode intensity in the whole system.
According to a second aspect of the present invention, there is provided a method for preparing a super-structured surface for humidity detection according to the first aspect, comprising the steps of:
S1, sequentially depositing a titanium layer, a gold layer and a transparent aluminum oxide layer on a clean silicon wafer by using a magnetron sputtering, electron beam evaporation or atomic layer deposition method;
s2, spin-coating a detection module material on the surface of the transparent alumina layer, and preparing a detection module through electron beam exposure or photoetching;
and S3, depositing a control module material on the surface of the transparent alumina layer by using a chemical vapor deposition process, and then preparing the control module by using a stripping process to obtain the super-structured surface for humidity detection.
In the preparation method provided by the invention, the stripping process omits the steps of sputtering chromium and the like in the hard mask etching process, and the process flow is shorter.
According to a third aspect of the present invention, there is provided another method for preparing a super-structured surface for humidity detection according to the first aspect, comprising the steps of:
SA, sequentially depositing a titanium layer, a gold layer and a transparent aluminum oxide layer on a clean silicon wafer by using a magnetron sputtering, electron beam evaporation or atomic layer deposition method;
SB, using chemical vapor deposition method to deposit contrast module material on the transparent alumina layer surface, spin coating PMMA resist on the contrast module material surface, exposing, using magnetron sputtering or electron beam evaporation to construct chromium film as hard mask, and forming contrast module by plasma etching;
and SC, directly preparing a detection module on the surface of the transparent alumina layer by using a detection module material by using an electron beam exposure method to obtain the super-structured surface.
In the preparation method provided by the invention, the hard mask is used for etching the control module, so that compared with the stripping process, the control module has more perfect appearance and higher processing repeatability.
A third aspect of the present invention provides a humidity sensor comprising an optical module for converting humidity change information into spectral information, the optical module comprising the above-described super-structured surface for humidity detection.
Preferably, the optical module further comprises a light source and a spectrometer.
Preferably, the humidity sensor further comprises a singlechip and a control circuit, wherein the singlechip is used for receiving and processing the output information of the optical module.
The working principle of the humidity sensor provided by the invention is that the light source irradiates on the super-structured surface, the super-structured surface absorbs light with specific wavelength under different humidity, the light is collected by the spectrometer after being reflected on the super-structured surface, the obtained spectrum information is analyzed to obtain corresponding environment humidity data, the environment humidity data is output by the spectrometer and then is received by the singlechip, and the singlechip processes and analyzes the data of the spectrometer and can upload the data to a subsequent host or cloud through the on-board antenna.
The invention has the beneficial effects that:
The super-structured surface and the humidity sensor using the super-structured surface provided by the invention have strong optical enhancement effect on the constrained BIC in the symmetrical protection continuous domain supported by the super-structured surface, can realize high-sensitivity humidity measurement, and ensure that the super-structured surface has response speed and recovery capability far smaller than those of an electric sensor while using smaller structural size. Meanwhile, the device adopts all-optical measurement, so that an external electrode is not needed, and the stability of the sensor in a complex environment is ensured.
The invention also provides a preparation method of the super-structured surface, which is simple to operate, and the super-structured surface and the humidity sensor prepared by the preparation method have the advantages of simple structure, small size, wide measurement range, high sensitivity, high response speed, strong environmental adaptability and high stability, and have wide application prospect.
Drawings
FIG. 1 is a schematic view of a super-structured surface according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a technical principle of detecting humidity on a super-structured surface according to an embodiment of the present invention;
FIG. 3 is a graph showing the variation of the field intensity of the super-structured surface according to example 1 of the present invention;
FIG. 4 is a schematic flow chart of the method for preparing a super-structured surface according to embodiment 2 of the present invention;
FIG. 5 is a schematic flow chart of a method for preparing a super-structured surface according to embodiment 3 of the present invention;
FIG. 6 is a schematic structural diagram of a humidity sensor according to an embodiment of the present invention;
FIG. 7 is a graph showing the reflection spectrum of the super-structured surface under different humidity conditions according to example 4 of the present invention;
Fig. 8 is a linear fit of the sensitivity of the super-structured surface provided in example 4 of the present invention according to different conditions.
Reference numerals illustrate:
1. a sensing layer; 2, a transparent alumina layer, 3, a gold mirror, 11, a comparison module, 12, a detection module, 31, a gold layer, 32 and a titanium layer.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of embodiments of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. It should be noted that the following examples are only for illustrating the implementation method and typical parameters of the present invention, and are not intended to limit the scope of the parameters described in the present invention, so that reasonable variations are introduced and still fall within the scope of the claims of the present invention.
It should be noted that endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and that such range or value should be understood to include values approaching such range or value. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Unless defined otherwise, all terms, symbols and other scientific terms used herein are intended to have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In some cases, terms with commonly understood meanings are defined herein for either clarity or for ease of reference, such definitions herein should not be construed to represent a significant departure from the conventional understanding in the art. The technical methods described or cited herein are generally well known to those skilled in the art and are employed by conventional methods. Unless otherwise indicated, the use of the kits and reagents, instruments, which are commercially available, are carried out according to the protocols and parameters given by the manufacturer.
In the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "left", "right", "inner", "outer", "front", "rear", "head", "tail", etc., are directions or positional relationships based on those shown in the drawings, or are directions or positional relationships conventionally put in use of the inventive product, are merely for convenience of describing the present invention and simplifying the description, and are not indicative or implying that the apparatus or element to be referred to must have a specific direction, be configured and operated in a specific direction, and thus should not be construed as limiting the present invention.
In order to solve the problems of slow response speed, narrow detection range and poor restorability and stability of an electrical humidity sensor in the prior art, the specific embodiment of the invention provides a super-structure surface for humidity detection, as shown in fig. 1, the super-structure surface comprises a sensing layer 1, a transparent alumina layer 2 and a gold mirror 3 which are arranged in a stacked manner, the sensing layer 1 comprises a comparison module 11 and a detection module 12, the arrangement of the comparison module 11 and the detection module 12 presents a binding state BIC in a continuous domain with symmetrical protection on an optical energy band, and the gold mirror 3 comprises a gold layer 31 and a titanium layer 32 which are arranged in a stacked manner from top to bottom.
In the above embodiment, the control module 11 and the detection module 12 are used for monitoring the environmental humidity in real time, the transparent alumina layer 2 is used for enhancing the overall sensing performance of the super-structure surface, and the principle of implementation is that the high-loss metal is separated from the low-loss photon structure as an isolation layer to improve the mode Q value, the gold layer 31 in the gold mirror 3 is used for improving the overall reflectivity of the structure as a reflection layer, and the titanium layer 32 is used as an adhesion layer for fixing the super-structure surface on a substrate in actual production activities.
In the above embodiment, the configuration of the contrast module 11 and the detection module 12 in the optical band is in a symmetrical protection continuous domain binding state, wherein the material of the detection module 12 is a humidity sensitive material, the material of the contrast module 11 is a humidity insensitive material, on the basis, when the humidity changes, the detection module 12 expands or contracts according to different humidities, the contrast module 11 will not change in shape, on the basis of this, the sensing layer 1 can change its symmetry by sensing the external humidity, when the humidity changes, the refractive index changes due to the change of the form of the detection module 12, so that the symmetry of the sensing layer 1 is broken in both directions of dielectric constant and geometry, the continuous binding state supported by the symmetrical structure at the point of the band Γ is converted into a quasi-continuous domain binding state in the asymmetric structure, so that the peak of the corresponding wavelength in the spectrum appears, and as the degree of the asymmetry of the external humidity changes the system is different, the continuous binding state in the quasi-continuous domain is converted into a quasi-domain state degree, and the quasi-continuous binding state in the different external humidity is different, and the Q-domain is converted into a quasi-continuous state with a high-domain loss due to the fact that the high-phase loss factor is generated in the high-quality of the system, and the high-quality loss is further due to the fact that the phase is converted in the quasi-domain is converted in the domain, and the relative-domain is more stable, and the loss is further due to the high-loss is generated. The super-structured surface provided by the embodiment is particularly suitable for detecting 35-90% humidity.
In a specific embodiment, the material of the detection module 12 may be a polymer, ceramic, or other material that is sensitive to humidity and whose morphology spectrum can be reversibly changed after reacting with water.
In a specific embodiment, the form of the detection module 12 may be any one of a grating structure, a waveguide structure, and a grating-waveguide composite structure.
In a specific embodiment, the material of the control module 11 is selected from glass, ceramic, high molecular polymer, and the like, which is insensitive to humidity and has no change in morphology spectrum after reacting with water.
In a specific embodiment, the form of the control module 11 is selected from any one of a grating structure, a square array and a circular disk array.
In a specific embodiment, the thickness of the transparent alumina layer 2 is 100nm or less, the thickness of the gold layer 31 is 100nm or more, and the thickness of the titanium layer 32 is 3-10 nm.
The specific embodiment of the invention also provides a preparation method of the super-structured surface for humidity detection, which specifically comprises the following steps:
s1, sequentially depositing a titanium layer 32, a gold layer 31 and a transparent aluminum oxide layer 2 on a clean silicon wafer by using a magnetron sputtering deposition method;
s2, directly preparing a polyvinyl alcohol grating on the surface of the transparent alumina layer 2 by using an electron beam exposure method;
And S3, depositing a silicon dioxide layer on the surface of the transparent aluminum oxide layer 2 by using a chemical vapor deposition method, and directly preparing a silicon dioxide grating by a stripping process to obtain the super-structured surface.
The method omits the steps of sputtering chromium and the like in the hard mask etching process through the stripping process, and has shorter process flow.
In a specific embodiment, the above-mentioned super-structured surface for humidity detection may be further manufactured by a manufacturing method comprising the steps of:
SA, sequentially depositing a titanium layer 32, a gold layer 31 and a transparent aluminum oxide layer 2 on a clean silicon wafer by using a magnetron sputtering deposition method;
SB, depositing a silicon dioxide layer on the surface of the transparent alumina layer 2 by using a chemical vapor deposition method, spin-coating PMMA (polymethyl methacrylate) resist on the surface of the silicon dioxide layer, exposing, constructing a chromium film on the silicon dioxide layer by using magnetron sputtering as a hard mask, and forming a silicon dioxide grating by plasma etching;
and SC, directly preparing a polyvinyl alcohol grating on the surface of the transparent alumina layer 2 by using an electron beam exposure method to obtain the super-structured surface.
Compared with the method using a stripping process, the contrast module has more perfect appearance and higher processing repeatability.
On the basis of the above super-structured surface for humidity detection, the specific embodiment of the present invention also provides a humidity sensor, which comprises a digital network module and an optical module, and the specific principle is shown in fig. 6.
In a specific embodiment, the optical module specifically includes a light source, the above-mentioned super-structured surface, a spectrometer and a control circuit, and the digital network module includes a single-chip microcomputer and a host computer or a cloud.
In a specific embodiment, the light source can emit incident light, the incident light irradiates the super-structured surface after microscopic focusing, collimation and polarization, at this time, the sensing layer 1 on the super-structured surface can change the form due to the change of the environmental humidity, on the basis, the reflection spectrum of the reflected light in the spectrometer can also change, the related data is received by the singlechip after being output by the spectrometer, and the singlechip can upload the data to a subsequent host or cloud through the on-board antenna after the data processing and analysis of the spectrometer.
The technical scheme of the invention is further described by specific examples.
Example 1
In this embodiment, the material used for the detection module 12 on the super-structured surface is polyvinyl alcohol, the shape of the detection module 12 is a grating structure, the material of the comparison module 11 is silicon dioxide, the shape of the comparison module 11 is a grating structure, in this embodiment, when the humidity is 90%, the grating pitch of the silicon dioxide grating is 710nm, the grating pitch of the polyvinyl alcohol grating is 710nm, and one period of 710nm comprises silicon dioxide grating strips and polyvinyl alcohol grating strips with a pitch of 46 nm. In this embodiment, the height of the grating bars of the silica grating is h1, h1=800 nm, the width is w1, w1=250 nm, the height of the grating bars of the polyvinyl alcohol grating is h2, h2=h1×β, and the width of the grating bars of the polyvinyl alcohol grating is w2=w1×β, where β is the relative shrinkage coefficient of the polyvinyl alcohol at a corresponding humidity relative to 90% humidity. This parameter increases with an increase in the ambient humidity, and when the ambient humidity is 90%, the β value is 1, and when the ambient humidity is 35%, the β value is 0.88864. In this example, the transparent alumina layer 2 had a thickness of 20nm, the gold layer 31 had a thickness of 150nm, and the titanium layer 32 had a thickness of 3nm.
Referring to fig. 2, the super-structured surface provided in this embodiment can change its own topological symmetry by sensing external humidity, and can open its optical energy band by adjusting the symmetry, specifically referring to a in fig. 2, the band gap applied to sensing is labeled as a continuous bound state 2. Referring to b in fig. 2, as the humidity changes from 35% to 90%, the band gap is opened, the supported continuous bound state is converted into the Quasi-continuous domain bound state, the spectrum shows a high Q peak, and a strong field enhancement occurs in the spectrum, and a specific field intensity diagram can be seen in fig. 3, as the band gap is opened, the structurally supported BIC (continuous bound state) is converted into Quasi-BIC (Quasi-continuous domain bound state), and the structural band gap can be changed because, on the basis, when the humidity changes, the polyvinyl alcohol grating expands or contracts for different humidity, the silicon dioxide grating does not change in morphology, on the basis, the polyvinyl alcohol grating and the silicon dioxide grating can change their own symmetry by sensing the external humidity, and on the basis, when the humidity changes, the symmetry of the silicon dioxide grating and the polyvinyl alcohol grating is broken in both the dielectric constant and the geometric direction due to the change of the refractive index of the polyvinyl alcohol, and the continuous bound state on the point of the energy band Γ supported by the symmetrical structure is converted into the Quasi-continuous bound state in the asymmetric structure. The method has the advantages that the peak of the corresponding wavelength on the spectrum appears, the degree of the bound state in the quasi-continuous domain is changed to be different along with the different degree of the asymmetry of the system caused by the change of the external humidity, the bound state in the quasi-continuous domain shows different Q factors under different external humidity, in addition, the high-quality factor mode can be subjected to larger loss in the structure due to the metal loss of the reflecting layer, so that the relative intensity of the mode is lower, in addition, due to the change of the structure, certain chromatic dispersion can be generated in the process of the bound state in the quasi-continuous domain, the external humidity can be defined through the mode Q factor, the mode spectral displacement and the mode intensity in the whole system, and the method is particularly suitable for humidity detection in the interval range of 35% -90%, and has the advantages of high reaction speed and strong recoverability.
Example 2
Referring to fig. 4, the present embodiment provides a method for preparing a super-structured surface for humidity detection, including the following steps:
a, after 3nm titanium is deposited as an adhesion layer by magnetron sputtering, 150nm gold is deposited as a reflecting layer;
b, performing magnetron sputtering on the surface of the gold layer 31 to form a transparent aluminum oxide layer 2 with the thickness of 20nm for enhancing reflection;
c, spin-coating polyvinyl alcohol with the thickness of 710nm on the surface of the transparent alumina;
d, after exposure is carried out on polyvinyl alcohol by using electron beam exposure, a PVA grating is prepared by using deionized water for development under the heating condition;
e, spin coating a layer of polymethyl methacrylate (PMMA) on the surface of the transparent alumina layer 2, wherein the thickness of the PMMA is larger than the height of the polyvinyl alcohol grating strips;
f, performing overlay on PMMA on the original basis by using electron beam exposure, and developing the PMMA by using MIBK;
g, depositing silicon dioxide with the thickness of 800nm by using chemical vapor deposition;
And h, removing residual PMMA by using acetone to prepare the SiO 2 grating and obtain the super-structured surface.
Example 3
Referring to fig. 5, this embodiment provides another preparation method of a super-structured surface for humidity detection, including the following steps:
a, after 3nm titanium is deposited as an adhesion layer by magnetron sputtering, 150nm gold is deposited as a reflecting layer;
b, magnetron sputtering transparent alumina with the thickness of 20nm on the surface of the gold layer 31 for enhancing reflection;
c, depositing silicon dioxide with the thickness of 800nm on the surface of the transparent alumina layer 2 by using chemical vapor deposition;
d, spin coating a layer of PMMA on the surface of the silicon dioxide;
e, exposing PMMA by using electron beam exposure and developing PMMA by using methyl isobutyl ketone (MIBK);
f, using magnetron sputtering to deposit a layer of thin chromium film as a mask;
Removing residual PMMA by using acetone;
Preparing a silicon dioxide grating by plasma etching;
acid washing to remove metal at the top of the silicon dioxide grating;
Spin-coating 800nm thick polyvinyl alcohol on the surface of the transparent alumina layer 2 under the high humidity condition;
k, after exposure is carried out on the polyvinyl alcohol by using electron beam exposure, deionized water is used for developing under the heating condition to prepare a polyvinyl alcohol grating;
And I, heating to remove water molecules in the polyvinyl alcohol grating, breaking the symmetry of the structure, and thus obtaining the super-structured surface.
Example 4
With the super-structured surface provided in example 1, the reflection spectrum of the super-structured surface was measured under the humidity condition of 35% -90%, and as a result, see fig. 7, the position of the peak in the super-structured surface spectrum in the humidity sensor gradually red-shifts with gradually decreasing relative intensity as the external humidity increases, see fig. 8, the linear fit of the super-structured surface by the relative intensity definition sensitivity at low humidity (s1=0.45/RH), the linear fit of the super-structured surface by the relative intensity definition sensitivity at high humidity (s2=2.63/RH), and the linear fit of the super-structured surface by the spectral displacement definition sensitivity at s=0.22 (nm/RH).
The super-structure surface and the humidity sensor provided by the specific embodiment of the invention are optical in nature, have the advantages of high response speed, high humidity sensitivity, high recovery speed and high stability, and are not influenced by environmental pH because the super-structure surface is optical in nature, and have the advantage of high stability.
Although the present disclosure is described above, the scope of protection of the present disclosure is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the disclosure, and these changes and modifications will fall within the scope of the invention.
Claims (10)
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