CN103543128A - Sensor based on self-supporting grating structure and preparation method thereof - Google Patents

Sensor based on self-supporting grating structure and preparation method thereof Download PDF

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Publication number
CN103543128A
CN103543128A CN201210238221.3A CN201210238221A CN103543128A CN 103543128 A CN103543128 A CN 103543128A CN 201210238221 A CN201210238221 A CN 201210238221A CN 103543128 A CN103543128 A CN 103543128A
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grating
self
dielectric
supporting
sensor
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谢常青
洪梅华
史丽娜
朱效立
李海亮
刘明
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Institute of Microelectronics of CAS
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Institute of Microelectronics of CAS
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Abstract

The invention discloses a sensor based on a self-supporting grating structure, which comprises: a self-supporting dielectric grating; and a metal grating formed on the dielectric grating; the sensor detects the refractive index change of a sample to be detected by utilizing a transmission absorption peak generated by guided wave resonance caused by the metal grating and the medium grating under the irradiation of plane waves. The self-supporting grating structure of the sensor is manufactured by a nano processing technology. The refractive index change of the sample to be detected is detected by utilizing a transmission absorption peak generated by guided wave resonance caused by the metal-dielectric grating under the vertical irradiation of light. The sensor adopts a periodic nano structure, has small volume and is easy to carry; meanwhile, the self-supporting grating structure is adopted, the manufacturing process and the testing method are simple, and the sensitivity is high.

Description

A kind of sensor based on self-supporting optical grating construction and preparation method thereof
Technical field
The present invention relates to sensor technical field, in particular, relate to a kind of sensor based on self-supporting optical grating construction and preparation method thereof.
Background technology
Detect immobilization biological chemical composition extremely important in biology, chemical fundamentals research and environmental monitoring, medical treatment and national defense safety.The sensor that detects immobilization biological chemical composition (bioactivators such as enzyme, antibody, antigen, microorganism, cell, tissue, nucleic acid), is widely used in the fields such as biotechnology, environmental monitoring, health care, Food Inspection and national defense safety.
At present, the sensor based on surface plasma body resonant vibration (SPR) technology is widely used with its higher sensitivity and high efficiency and development fast, is the main tool that characterizes chemistry and bio-molecular interaction.The ultimate principle of spr sensor is by the variation of recording surface plasma resonance angle or resonant wavelength, realizes the detection to metal surface testing liquid analyte refractive index.Compare with the sensor of other type, sensor based on surface plasma body resonant vibration carrys out recognition sample by detecting the change of sample refractive index, do not need fluorescence labels or other labels, can carry out original position, harmless and unmarked detection to sample, so surface plasma resonance sensor is free of contamination high sensor.
Typical spr sensor is prism-type, comprise prism structure, as Kretschmann prism structure, and the metal film plating on prism structure, such as Au, Ag film etc., testing sample is positioned on metal film, p polarized light incides the interface of prism and metal film at a certain angle through prism, for certain incident angle and optical wavelength, prism provides the coupling of the wave vector between incident electromagnetic wave and surface plasma, and the sensitivity of the spr sensor of prism-type is higher.Yet the volume of prism structure own is large, cost is high, cause bulky, the complex structure of the spr sensor of prism-type, cost high, be conventionally applicable to detect in laboratory, not portable, not easy of integration yet.
On the other hand, trace gas detection is extremely important in fields such as environmental protection, safety, industrial process control and meteorologies.The commercial gas sensor that has at present several types, for example catalytic colorimetry gas sensor, electrochemical gas sensor and optical gas sensor.In all gas sensor, optical sensor does not interact owing to relying on galvanochemistry, so be the most accurately and reliably.The most frequently used optical sensor is infrared absorption spectrum sensor, and the variation that this class sensor is generally measured refractive index by the change in location of absorption peak on the transmitted spectrum of measurement gas, that is to say, the imaginary part of measurement gas refractive index.The major advantage of infrared absorption spectrum sensor is to measure nearly all gas, and major defect is that volume is large, complex structure, and expensive owing to needing infrared eye, high-resolution spectrometer and very long air chamber to strengthen absorption.
For the complicacy that reduces to measure, improve sensitivity, and reduce costs, people utilize MEMS (micro electro mechanical system), developed various without tag sensor technology, for example surface plasma resonance and guided wave resonance sensing technology.Meanwhile, the miniaturization of biosensor analysis system and portability are being even more important aspect biomedical and national defence.Aspect microminiaturized and high sensitivity, the sub-crystal probe of all-dielectric optically based on guided wave resonance has huge potentiality.
In a typical photonic crystal sensors, a branch of plane wave incides on photonic crystal panel, and the structural parameters of appropriate design photonic crystal can inspire the long-life radiation mode of local in photonic crystal panel.This pattern is extremely responsive to the structural parameters of photonic crystal and material, and this is that we utilize photonic crystal to make the main cause of sensor.In actual applications, by measuring the movement of crest frequency, obtain the subtle change of refractive index.
Summary of the invention
(1) technical matters that will solve
For solving above-mentioned one or more technical matterss, the invention provides a kind of sensor based on self-supporting optical grating construction and preparation method thereof, to realize the detection to gaseous state or liquid sample, obtain high sensitivity, and be easy to integrated and manufacture, reduce costs.
(2) technical scheme
According to an aspect of the present invention, the invention provides a kind of sensor based on self-supporting optical grating construction, comprising: the dielectric grating of self-supporting; And be formed at the metal grating on this dielectric grating; Wherein this sensor is to utilize transmission absorption peak that guided wave resonance that this metal grating and this dielectric grating cause under plane wave illumination produces to survey the variations in refractive index of testing sample.
In such scheme, this dielectric grating and this metal grating are periodic one-dimensional grating structure, and its cycle is between between 500 nanometers to 5 micron.
In such scheme, this metal grating is made on this dielectric grating, and the dutycycle of this dielectric grating and this metal grating is identical, and its dutycycle is between 65% to 95%.
In such scheme, the dielectric material adopting in this dielectric grating is silicon nitride, silit or polyimide material, and the metal material that this metal grating adopts is gold or silver-colored.
In such scheme, the grizzly bar height of this dielectric grating is between between 200 nanometers to 5 micron, and the grizzly bar height of this metal grating is between between 20 nanometers to 2 micron.
According to another aspect of the present invention, the present invention also provides a kind of preparation method of the sensor based on self-supporting optical grating construction, the method comprises: the dielectric film that forms self-supporting on the silicon chip of polishing, on this dielectric film, make metal grating, and etch dielectric grating under the sheltering of this metal grating.
In such scheme, the described dielectric film that forms self-supporting on the silicon chip of polishing, comprise: using plasma strengthens chemical gaseous phase depositing process and on silicon chip, deposits certain thickness silit or silicon nitride film, or by the certain thickness polyimide solution of spin coating on silicon chip, by baking oven, toast the dry rear Kapton that obtains; Adopt wet etching method from the silicon substrate back side, to remove the silicon substrate of graph area, form silicon nitride or silit or the Kapton structure of self-supporting.
In such scheme, describedly on this dielectric film, form metal grating, comprising: adopt electron beam lithography and electroplating technology to make metal grating in the silicon nitride of self-supporting or silit or Kapton structure.
In such scheme, describedly under the sheltering of metal grating, etch dielectric grating, comprise: adopt inductively coupled plasma lithographic technique that the dielectric thin-film material etching below this metal grating space is saturating, leave metal grating and shelter lower dielectric material, the dielectric grating of formation self-supporting; The dielectric grating of self-supporting and metal grating form the sensor based on self-supporting optical grating construction jointly.
According to another aspect of the present invention, the present invention also provides a kind of system of testing liquid state or gaseous sample refractive index, and this system comprises the sensor of light source, self-supporting optical grating construction, liquid state to be measured or gaseous sample and photo-detector; During test, the sensor of this self-supporting optical grating construction is soaked among this liquid state to be measured or gaseous sample; The detection light being sent by light source impinges perpendicularly on the sensor of this self-supporting optical grating construction, coupling generation guided wave resonance due to light and optical grating construction, guided wave resonance pattern and liquid state to be measured or gaseous sample interact, and make by the transmitted light generation transmission absorption peak of the sensor of this self-supporting optical grating construction; Photo-detector detects the position of this absorption peak and realizes the measurement to liquid state to be measured or gaseous sample refractive index.
(3) beneficial effect
Compared with prior art, the present invention has following beneficial effect:
(1) sensor based on self-supporting optical grating construction provided by the invention and preparation method thereof, the sensor of realizing by the grating of micro nano structure, simple in structure, lower to processing technology requirement, compatible with traditional semiconductor technology, be easy to integrated.
(2) sensor based on self-supporting optical grating construction provided by the invention and preparation method thereof, adopt the cycle nanostructured of grating and the coupling of the light wave of vertical incidence to excite guided wave resonance, produce resonance absorbing peak, for surveying the variation of sample refractive index, highly sensitive, method of testing is simple, easily realizes, and device architecture volume is little, is easy to carry about with one.
(3) sensor based on self-supporting optical grating construction provided by the invention and preparation method thereof, the position of the resonance absorbing peak that the grating of different cycles produces is different, researchist can make the grating of different cycles size as required, meets the measurement in different wave length situation.
Accompanying drawing explanation
Fig. 1 is the regional area structural drawing of the sensor based on self-supporting optical grating construction provided by the invention;
Fig. 2 is the vertical view according to the sensor based on self-supporting optical grating construction of the embodiment of the present invention;
Fig. 3 is the manufacturing process process flow diagram of the sensor based on self-supporting optical grating construction according to the embodiment of the present invention.
Fig. 4 is the sample test system schematic according to the sensor based on self-supporting optical grating construction of the embodiment of the present invention;
Fig. 5 is that the sensor based on self-supporting optical grating construction is tested the transmission spectrum obtaining to the gas of different refractivity according to the embodiment of the present invention;
Fig. 6 is the transmission absorption peak position of the sensor based on self-supporting optical grating construction according to the embodiment of the present invention and the relation of testing sample refractive index;
Fig. 7 is transmission absorption peak position and the relation in grating cycle of the sensor based on self-supporting optical grating construction according to the embodiment of the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
The invention discloses a kind of sensor based on self-supporting optical grating construction and preparation method thereof.This sensor comprises: the dielectric grating of self-supporting; And be formed at the metal grating on this dielectric grating; Wherein this sensor is to utilize transmission absorption peak that guided wave resonance that this metal grating and this dielectric grating cause under plane wave illumination produces to survey the variations in refractive index of testing sample.
Wherein, this dielectric grating and this metal grating are periodic one-dimensional grating structure, and its cycle is between between 500 nanometers to 5 micron.This metal grating is made on this dielectric grating, and the dutycycle of this dielectric grating and this metal grating is identical, and its dutycycle is between 65% to 95%.The dielectric material adopting in this dielectric grating is silicon nitride, silit or polyimide material, and the metal material that this metal grating adopts is gold or silver-colored.The grizzly bar height of this dielectric grating is between between 200 nanometers to 5 micron, and the grizzly bar height of this metal grating is between between 20 nanometers to 2 micron.
Sensor provided by the invention adopts cycle nanostructured, and volume is little, is easy to carry about with one; Adopt self-supporting optical grating construction, manufacture craft and method of testing are simple simultaneously, and susceptibility is high.
Based on the above-mentioned sensor based on self-supporting optical grating construction, the present invention also provides a kind of preparation method of the sensor based on self-supporting optical grating construction, and the method comprises: the dielectric film that forms self-supporting on the silicon chip of polishing; On this dielectric film, make metal grating; And etch dielectric grating under the sheltering of this metal grating.The self-supporting optical grating construction of this sensor is to be made by nanofabrication technique.
Wherein, the described dielectric film that forms self-supporting on the silicon chip of polishing, comprise: using plasma strengthens chemical gaseous phase depositing process and on silicon chip, deposits certain thickness silit or silicon nitride film, or by the certain thickness polyimide solution of spin coating on silicon chip, by baking oven, toast the dry rear Kapton that obtains; Adopt wet etching method from the silicon substrate back side, to remove the silicon substrate of graph area, form silicon nitride or silit or the Kapton structure of self-supporting.
Describedly on this dielectric film, form metal grating, comprising: adopt electron beam lithography and electroplating technology to make metal grating in the silicon nitride of self-supporting or silit or Kapton structure.
Describedly under the sheltering of metal grating, etch dielectric grating, comprise: adopt inductively coupled plasma lithographic technique that the dielectric thin-film material etching below this metal grating space is saturating, leave the dielectric material of metal grating under sheltering, form the dielectric grating of self-supporting; The dielectric grating of self-supporting and metal grating form the sensor based on self-supporting optical grating construction jointly.
For the scheme that the present invention is proposed is carried out experimental verification, the grating that to have designed one-period in experiment be 750nm, the width of grating grizzly bar is 95nm, the material of metal grizzly bar is gold, thickness is 200nm, the material of medium grizzly bar is silicon nitride, and thickness is 500nm, and the partial schematic diagram of grating as shown in Figure 1.Fig. 2 is the vertical view according to the sensor based on self-supporting optical grating construction of the embodiment of the present invention, and zone line is grating region, and size is 1mm * 1mm, and the grating in this region is grating shown in Fig. 1 after amplifying, and surrounding is for supporting the propping material of grating grizzly bar.
Fig. 3 is the manufacturing process process flow diagram of the sensor based on self-supporting optical grating construction according to the embodiment of the present invention.Manufacturing process comprises:
Step S1: using plasma strengthens chemical gaseous phase depositing process and deposit certain thickness carborundum films on silicon chip, and carborundum films thickness is 500nm;
Step S2: adopt wet etching method, such as adopting 33% potassium hydroxide solution, remove the silicon substrate of graph area from the silicon substrate back side, size is 1mm * 1mm, forms self-supporting silicon nitride film structure;
Step S3: adopt beamwriter lithography and developing technique, by being spin-coated on resist on membrane structure and producing the groove of 95nm width, then electroplate the gold of 200nm thickness in groove the inside by golden electroplating technology, obtain the golden grizzly bar of 200nm thickness after resist removes photoresist;
Step S4: adopt inductively coupled plasma lithographic technique that the silicon nitride film structure etching below metal grating space is saturating, leave the silicon nitride material of metal grating under sheltering, form the silicon nitride grating grizzly bar of 500nm thickness below metal grizzly bar.
Fig. 4 is the sample test system schematic of the sensor based on self-supporting optical grating construction according to the embodiment of the present invention.As shown in Figure 4, this sample test system comprises light source, sensor, liquid state to be measured or gaseous sample, photo-detector.During specimen, sensor is soaked among liquid state to be measured or gaseous sample; The detection light being sent by light source impinges perpendicularly on self-supporting optical grating construction sensor; Due to the coupling generation guided wave resonance of light and optical grating construction, guided wave resonance pattern and liquid state to be measured or gaseous sample interact, and make to produce transmission absorption peak by the transmitted light of sensor; By photo-detector, detect the position measurement liquid state to be measured of absorption peak or the refractive index of gaseous sample.
Fig. 5 is that the sensor based on self-supporting optical grating construction is tested the transmission spectrum obtaining to the gas of different refractivity according to the embodiment of the present invention.As shown in Figure 5, coupling generation guided wave resonance due to light and optical grating construction, guided wave resonance pattern and liquid state to be measured or gaseous sample interact, and make to produce transmission absorption peak by the transmitted light of sensor, and the position of absorption peak is directly proportional to the refractive index of testing sample.The refractive index susceptibility of sensor is:
S ( λ , n 1 , n 2 ) = lim Δn → 0 λ ( n 1 ) - λ ( n 2 ) n 1 - n 2 = 759.78 - 752.57 1.01 - 1.00 ≈ 721 nm / RIU
Fig. 6 is the transmission absorption peak position of the sensor based on self-supporting optical grating construction according to the embodiment of the present invention and the relation of testing sample refractive index, as can be seen from Figure 6, in the present invention, the transmission absorption peak position of the sensor based on self-supporting optical grating construction and testing sample refractive index are linear.
Fig. 7 is transmission absorption peak position and the relation in grating cycle of the sensor based on self-supporting optical grating construction according to the embodiment of the present invention, transmission absorption peak position and the grating cycle of the sensor based on self-supporting optical grating construction in visible the present invention are proportional, simultaneously, in grating cycle increase situation, the susceptibility of the sensor obtaining is also higher.When the grating cycle is 3000nm, the susceptibility of sensor becomes 2952nm/RIU.Researchist can make the grating of different cycles size as required, meets the measurement in different wave length and varying sensitivity situation.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (10)

1. the sensor based on self-supporting optical grating construction, is characterized in that, comprising:
The dielectric grating of self-supporting; And
Be formed at the metal grating on this dielectric grating;
Wherein, this sensor is to utilize transmission absorption peak that guided wave resonance that this metal grating and this dielectric grating cause under plane wave illumination produces to survey the variations in refractive index of testing sample.
2. the sensor based on self-supporting optical grating construction according to claim 1, is characterized in that, this dielectric grating and this metal grating are periodic one-dimensional grating structure, and its cycle is between between 500 nanometers to 5 micron.
3. the sensor based on self-supporting optical grating construction according to claim 1, is characterized in that, this metal grating is made on this dielectric grating, and the dutycycle of this dielectric grating and this metal grating is identical, and its dutycycle is between 65% to 95%.
4. the sensor based on self-supporting optical grating construction according to claim 1, is characterized in that, the dielectric material adopting in this dielectric grating is silicon nitride, silit or polyimide material, and the metal material that this metal grating adopts is gold or silver-colored.
5. the sensor based on self-supporting optical grating construction according to claim 1, is characterized in that, the grizzly bar height of this dielectric grating is between between 200 nanometers to 5 micron, and the grizzly bar height of this metal grating is between between 20 nanometers to 2 micron.
6. a preparation method for the sensor based on self-supporting optical grating construction, is characterized in that, the method comprises:
On the silicon chip of polishing, form the dielectric film of self-supporting;
On this dielectric film, make metal grating; And
Under the sheltering of this metal grating, etch dielectric grating.
7. the preparation method of the sensor based on self-supporting optical grating construction according to claim 6, is characterized in that, the described dielectric film that forms self-supporting on the silicon chip of polishing, comprising:
Using plasma strengthens chemical gaseous phase depositing process and on silicon chip, deposits certain thickness silit or silicon nitride film, or by the certain thickness polyimide solution of spin coating on silicon chip, by baking oven, toasts the dry rear Kapton that obtains;
Adopt wet etching method from the silicon substrate back side, to remove the silicon substrate of graph area, form silicon nitride or silit or the Kapton structure of self-supporting.
8. the preparation method of the sensor based on self-supporting optical grating construction according to claim 6, is characterized in that, describedly on this dielectric film, forms metal grating, comprising:
Adopt electron beam lithography and electroplating technology to make metal grating in the silicon nitride of self-supporting or silit or Kapton structure.
9. the preparation method of the sensor based on self-supporting optical grating construction according to claim 6, is characterized in that, describedly under the sheltering of this metal grating, etches dielectric grating, comprising:
Adopt inductively coupled plasma lithographic technique that the dielectric thin-film material etching below this metal grating space is saturating, leave metal grating and shelter lower dielectric material, the dielectric grating of formation self-supporting; The dielectric grating of self-supporting and metal grating form the sensor based on self-supporting optical grating construction jointly.
10. a system of testing liquid state or gaseous sample refractive index, is characterized in that, this system comprises the sensor of the self-supporting optical grating construction described in light source, claim 1 to 5, liquid state to be measured or gaseous sample and photo-detector;
During test, the sensor of this self-supporting optical grating construction is soaked among this liquid state to be measured or gaseous sample; The detection light being sent by light source impinges perpendicularly on the sensor of this self-supporting optical grating construction, coupling generation guided wave resonance due to light and optical grating construction, guided wave resonance pattern and liquid state to be measured or gaseous sample interact, and make by the transmitted light generation transmission absorption peak of the sensor of this self-supporting optical grating construction; Photo-detector detects the position of this absorption peak and realizes the measurement to liquid state to be measured or gaseous sample refractive index.
CN201210238221.3A 2012-07-10 2012-07-10 Sensor based on self-supporting grating structure and preparation method thereof Pending CN103543128A (en)

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CN105651737A (en) * 2015-12-24 2016-06-08 江苏双仪光学器材有限公司 Metal laminated medium sub-wavelength grating-based biological sensing chip
CN106646680A (en) * 2016-11-14 2017-05-10 四川大学 One-way wave guide device based on composite structures
CN109001157A (en) * 2018-06-22 2018-12-14 江南大学 A method of refractive index sensing is realized based on duplex surface plasma resonance
CN109001157B (en) * 2018-06-22 2020-07-07 江南大学 Method for realizing refractive index sensing based on dual surface plasmon resonance
CN111398217A (en) * 2019-06-05 2020-07-10 江西师范大学 High-quality plasmon optical sensor and preparation method thereof
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CN111948175A (en) * 2020-08-05 2020-11-17 浙江大学 high-Q high-FoM metal medium auxiliary GMR refractive index sensing chip

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Application publication date: 20140129