CN112275333A - Sensing chip based on FP laser and metal array structure and preparation method thereof - Google Patents

Sensing chip based on FP laser and metal array structure and preparation method thereof Download PDF

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CN112275333A
CN112275333A CN202011075860.3A CN202011075860A CN112275333A CN 112275333 A CN112275333 A CN 112275333A CN 202011075860 A CN202011075860 A CN 202011075860A CN 112275333 A CN112275333 A CN 112275333A
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laser
layer
sensing
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袁浚
王文杰
廖明乐
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Institute of Electronic Engineering of CAEP
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/0014—Monitoring arrangements not otherwise provided for
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/06—Auxiliary integrated devices, integrated components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/06—Auxiliary integrated devices, integrated components
    • B01L2300/0627—Sensor or part of a sensor is integrated

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  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
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Abstract

The invention discloses a sensing chip based on an FP laser and a metal array structure and a preparation method thereof, belonging to the technical field of optoelectronic devices and sensing. The chip is prepared by growing a medium isolation layer on the light emergent end face of an FP laser, manufacturing a metal array structure for biosensing on the end face of the medium isolation layer by adopting micro-nano processing technology such as focused ion beams, and integrating a micro-flow channel manufactured by PDMS (polydimethylsiloxane) with the chip by adopting the micro-fluidic technology to realize the sensing packaging of the chip so as to carry out sensing detection; in the structure, the intensity of the emergent wavelength of the FP laser is influenced by the refractive index change of the surface of the metal array structure, a sample to be detected is introduced into the microfluidic channel, and the sample to be detected can be sensed by testing the change of the emergent light intensity. The invention achieves the miniaturization of the sensing equipment by integrating the laser and the detector and highly integrating the sensing sensitive unit and the sensing optical part.

Description

Sensing chip based on FP laser and metal array structure and preparation method thereof
Technical Field
The invention relates to the technical field of photoelectronic devices and sensing, in particular to a sensing chip based on an FP laser and a metal array structure and a preparation method thereof.
Background
With the improvement of living standard, people pay more and more attention to their health status, and whether to detect body indexes timely and accurately becomes an important problem to be solved urgently in the medical field. Meanwhile, the destruction of the ecological environment also makes people more and more concern about the environment and pay attention to the environmental protection, so that the development of a portable sensor with low cost and high sensitivity to realize the real-time monitoring of the ecological environment becomes a research hotspot in the current sensing field. The sensing chip prepared by the semiconductor processing technology has the advantages of small volume, high sensitivity, low manufacturing cost and the like, and can be widely applied to the fields of biomedicine, environmental monitoring and the like.
The surface plasma excited on the surface of the metal array structure prepared by the semiconductor processing technology is very sensitive to the change of the surface characteristics of metal or dielectric medium, and is suitable for representing the related properties of the metal surface flatness, adsorbates and the like. The sensor has the advantages of small sample consumption, high sensitivity, strong anti-interference capability and the like, and is widely applied to the fields of chemistry and biological sensing.
In the surface plasma sensing of the metal array, except that the wavelength detection needs a broad spectrum light source, the other detection technologies can adopt laser light sources. The semiconductor laser has the advantages of small volume, low cost, low power consumption, long service life, good stability and the like, is particularly suitable for miniaturization of detection equipment, and currently, researchers select the semiconductor laser as a light source of a surface plasma sensing chip.
The FP (Fabry-perot) laser, as a new type of semiconductor laser, has the characteristics of low cost, high light output power, etc., and is widely used in short-distance optical fiber communication and sensing applications. At present, laser-based optical sensors have been used in the fields of optical navigation tracking, gas sensing monitoring and the like, but there is no method and integrated chip for detecting trace substances in the fields of biology, chemistry and medicine in real time by integrating FP lasers with high light output power with metal array structures.
Disclosure of Invention
The invention aims to provide a sensing chip based on an FP laser and a metal array structure and a preparation method thereof, which utilize the characteristics of low cost, small volume and high light output power of the FP laser to realize the miniaturization of the sensing structure by mainly integrating the FP laser and the metal array structure, and the prepared sensing chip can be used for detecting biological samples and environmental indexes and has wide application space.
In order to achieve the above object, the technical solution of the present invention is as follows:
sensing chip based on FP laser instrument, its characterized in that: the device comprises a FP laser at the lower part and a metal array structure at the upper part, wherein a medium isolation layer is arranged on the light-emitting end face of the FP laser, a PDMS (polydimethylsiloxane) shell is arranged on the upper end face of the medium layer, the PDMS shell comprises a side wall and a top surface, a cavity formed by the side wall, the top surface and the upper end face of the medium layer is a microfluidic channel, a sample injection port and a sample outflow port are arranged on the top surface, and the sample injection port and the sample outflow port are positioned at two ends of the microfluidic channel; in the micro-flow channel, a metal array structure is arranged on the upper end face of the medium layer.
Furthermore, the dielectric isolation layer can be made of insulating dielectric materials such as a silicon dioxide layer or a silicon nitride layer, and can effectively isolate the light-emitting surface of the FP laser from the metal array structure, so that the light-emitting surface and the metal array structure do not interact with each other.
Further, the metal array structure is a sensing layer of a sensing chip, and the structure may be: metal gratings, metal lattices, and the like.
Furthermore, the PDMS shell is a cylindrical structure with an opening at the bottom. Wherein, the PDMS shell can be a cuboid tubular structure.
Further, the sensing chip based on the FP laser is arranged below the detector, and the top surface of the PDMS shell is opposite to the lower side of the detector.
Further, the sample injection port and the sample outflow port are located at both ends of the top surface of the PDMS casing.
The preparation method for preparing the sensing chip based on the FP laser is characterized by comprising the following steps:
(1) growing a film on the light emergent end face of the FP laser, wherein the film is a medium isolating layer;
(2) evaporating a layer of metal film on the medium isolation layer, and then manufacturing the metal film into a metal array structure by utilizing a micro-nano processing technology;
(3) a PDMS film with an opening at the bottom is manufactured by a PDMS mold turning technology to form a PDMS shell with a cylindrical structure;
(4) punching a hole at the top of the PDMS shell to form a sample injection port and a sample outflow port;
(5) and on the medium isolation layer, bonding the outer edges of the PDMS shell and the upper surface of the medium isolation layer after corona treatment to manufacture the sensing chip, wherein a cavity between the PDMS shell and the upper surface of the medium isolation layer is matched with the sample injection port and the sample outflow port to form a micro-flow channel.
Further, the dielectric film isolation layer in step (1) may be grown by using a dielectric film growth technique such as chemical vapor deposition or magnetron sputtering.
Further, the micro-nano processing technology in the step (2) can adopt a focused ion beam direct writing technology or an electron beam exposure technology to manufacture a metal array structure for biosensing. The structure is prepared by firstly growing a noble metal film (such as Au, Ag and the like) with the thickness of dozens of nanometers on a medium isolating layer and then utilizing a micro-nano processing technology.
The metal array structure for sensing needs special design, so that the metal array structure has an obvious transmission peak at the light-emitting wavelength of the FP laser, and when liquid to be detected is introduced into the metal array structure, the light intensity of the metal array structure needs to be obviously changed so as to realize detection of related substances. In the selection of a specific metal array structure, the design can be carried out by a three-dimensional time domain finite difference method, and the structures such as a grating, a circular hole, a dot matrix and the like with high sensitivity and excellent performance are selected, and the size of the structures is generally dozens of nanometers.
Further, the sample injection port and the sample outflow port in the step (4) are formed on the top of the PDMS casing, and are respectively prepared at two ends of the microfluidic channel by using a hole puncher. During installation, the L-shaped steel pipes are respectively inserted into the sample injection port and the sample outflow port so as to realize the connection between the rubber pipe and the microfluidic channel.
Further, the microfluidic channel in step (3) is transferred to PDMS by using an over-mold technique. PDMS has no absorption peak in the light-emitting band of FP laser, and is a transparent film. The height of the microfluidic channel is generally dozens of microns, and the test solution can meet the test requirement only by dozens of microliters, so that the dosage of the required sample to be tested is very small. Furthermore, PDMS is very biocompatible and does not have side effects on the test samples.
Further, in the step (5), the surfaces of the PDMS and the chip are treated by a corona method, so that irreversible bonding is formed between the two surfaces, and a complete novel sensing chip is further combined. And injecting a sample to be detected by a micro-flow pump, wherein the injection flow and the flow rate can be very accurately controlled by the method, and accurate real-time monitoring is realized. In addition, the static monitoring of the chip can be realized by injecting a sample through a medical injector.
After the sensing packaging of the sensing chip is realized, the sensing chip enters the sensing chip through the micro-flow channel of the PDMS shell in sensing detection, and the change of the light intensity of the FP laser before and after the solution to be detected is introduced is tested by using the optical power meter to realize the chip sensing.
Compared with the existing sensor based on the FP laser, the technical scheme has the following beneficial effects:
1. the invention realizes the integration of the FP laser and the metal array sensing structure, realizes the miniaturization of the sensing structure, and can further integrate the detector and the chip in the future, so that the construction of a lab-on-a-chip based on the FP laser becomes possible.
2. Due to the integration of the FP laser and the metal array structure, the size of the sensing chip is further reduced, and the stability and reliability of the device are improved.
3. The FP laser can be prepared by a semiconductor planar process, and other parts of the chip can also be prepared by the semiconductor process, so that the chip can be finally prepared by the planar semiconductor process.
4. The metal array structure integrated on the end face of the FP laser can be used for detecting biological samples and environmental indexes, and has wide application space. In addition, different structural parameters can be designed according to different samples to be detectedThe metal array structure realizes high-sensitivity detection of the object to be detected by effectively controlling the transmissivity of the metal array structure, and the expected detection precision can reach 10-8。
5. The invention can be used for detecting trace substances in the fields of biology, chemistry and medicine, and has the advantages of real-time and rapid detection and the like.
Drawings
Fig. 1 is a schematic cross-sectional structure diagram of a sensor chip of the present invention.
Fig. 2 is a schematic top view of the surface plasmon resonance sensor apparatus according to embodiment 2.
FIG. 3 is the transmission spectrum of the gold slit array in example 2 in different refractive index media.
FIG. 4 is a transmission spectrum of the gold slit array in example 2 at about 842.33 nm.
FIG. 5 is a graph of the transmission intensity at 842.33nm in the refractive index of different media in example 2 and its linear fit to the refractive index.
Wherein: 1 is a sample injection port, 2 is a sample outflow port, 3 is a microfluidic channel, 4 is a gold slit array, and 5 is SiO2Membrane, 6 for FP laser, 7 for PDMS shell, 8 for detector.
Detailed Description
In order to more clearly show the working principle and the working process of the present invention, a novel surface plasmon resonance sensor chip based on an FP laser and a gold slit grating is taken as an example and is described with reference to the accompanying drawings.
Example 1
The sensing chip based on the FP laser comprises the FP laser and a metal array structure. The method comprises the following steps: a medium isolation layer is arranged on the light-emitting end face of the FP laser, a PDMS shell is arranged on the upper end face of the medium layer, the PDMS shell comprises a side wall and a top surface, a cavity formed by the side wall, the top surface and the upper end face of the medium layer is a microfluidic channel, and a sample injection port and a sample outflow port are arranged on the top surface; in the micro-flow channel, a metal array structure is arranged on the upper end face of the medium layer.
Example 2
Based on the sensing chip structure of embodiment 1, the chip structure shown in fig. 1 specifically includes:
the lasing wavelength of the FP laser 6 is 842.33 nm.
The dielectric isolation layer is made of SiO2Growth value of, SiO2The thickness of the film was 300 nm.
The metal array structure is a gold slit array, wherein: the metal is gold, the period of the gold grating is 600nm, the slit width of the gold grating is 80nm, and the thickness of the gold film is 50 nm.
The sensing chip structure shown in fig. 1 sequentially comprises the following manufacturing steps:
growing a layer of SiO with the thickness of 300nm on the light-emitting end face of an FP laser 6 with the laser wavelength of 842.33nm2And (5) a membrane.
In SiO2A gold film with the thickness of 50nm is evaporated on the film 5, and the gold film is manufactured into a gold slit array 4 with the period of 575nm and the slit width of 80nm by utilizing a focused ion beam direct writing technology.
A PDMS film is prepared using an over-mold technique, and a sample injection port 1 and a sample outflow port 2 are formed by punching through a punch. Wherein the sample injection port 1 and the sample outflow port 2 have a diameter of 1 mm.
Carrying out corona treatment on the outer edges of the PDMS shell 7 and the upper surface of the medium isolation layer, and then bonding to manufacture a complete sensing chip, wherein a micro-flow channel 3 is formed in the middle; the sample to be measured can be introduced into and discharged from the microfluidic channel 3 through the sample injection port 1 and the sample outflow port 2.
When the invention works: 842.33nm laser emitted by FP laser 6 passes through SiO2Film 5, SiO2The film 5 has substantially no loss of the emitted laser light and has the function of isolating the light-emitting surface of the FP laser from the gold slit array 4 so that the FP laser 6 and the gold slit array 4 do not interact with each other. The intensity and wavelength of the transmission peak of the gold slit array 4 in the medium with different refractive indexes are changed correspondingly, as shown in fig. 3. Especially at 842.33nm, as the refractive index of the medium in the microfluidic channel 3 changes, the transmission intensity changes accordingly. As shown in fig. 4, the transmission peak of the gold slit array 4 changes at medium refractive indices of 1.333,1.343,1.353,1.363, and 1.373, 843.2The transmission intensity at 2nm is also different. And the PDMS shell 7 has no large loss to 842.33nm light, and the change of the medium refractive index in the micro-flow channel 3 can be sensed by testing the intensity of emergent light.
As shown in fig. 5, when the refractive indexes of the media in the microfluidic channel 3 are 1.333,1.343,1.353,1.363, and 1.373, the transmission intensities thereof are 0.726,0.563,0.353,0.148, and 0.041 of the light intensity emitted from the FP laser 6, respectively. A linear fit of the intensity and refractive index gave a slope of-18.2. In the range of refractive index 1.333-1.373, the intensity of the emitted light detected at 843.22nm decreased by 18.2% of the emitted light intensity every time the refractive index increased by 0.01. The intensity of the emitted light of the FP laser 6 is 1W, and the detection accuracy of the laser detector is 1 μ W, i.e. a change in emitted light intensity in parts per million can be detected. A change in luminescence intensity in parts per million corresponds to a change in refractive index of about 10-8It has higher sensitivity and higher detection limit.
For the sensor chip manufactured as described above, the height of the microfluidic channel 3 is 70 μm, and the sample to be measured can be measured generally only by the amount of tens of microliters. By utilizing the good biocompatibility of PDMS, no side effect is caused to a test sample. After the sample to be tested enters the microfluidic channel 3, the sample to be tested is contacted with the upper surface of the gold slit array 4, the medium refractive index of the upper surface is changed, and the refractive index of the sample to be tested can be obtained by testing the intensity of emergent light.
Besides the change of the refractive index of the test sample, the sensing chip can also sense trace amount of biomolecules. Introducing dithiodiglycolic acid into the microchannel to form a gold-sulfur bond with gold; then introducing crosslinking agents such as EDC/NHS and the like to bond with dithiodiglycolic acid to form a layer of hydroxyl on the surface of the gold; and finally, introducing biomolecules, wherein the biomolecules comprise antigens, antibodies, biotin, proteins or nucleic acid molecules and the like, and can be bonded with hydroxyl to form a biomolecule layer on the surface. The biomolecular layer is bonded on the surface of the gold slit array, the refractive index of the surface of the gold slit array is changed, the refractive index change caused by the biomolecular layer is larger than the lowest detection limit of the sensing chip, and the biomolecular layer can be tested by a sensing system.
The above examples are only examples for illustrating the method, and are not all examples for realizing the method of the present invention, and the FP lasers with different emission wavelengths only need to correspond to the metal nanostructure having a transmission peak at the emission wavelength, so that the detection of the solution refractive index and the biomolecule can be realized by a similar method.

Claims (10)

1. Sensing chip based on FP laser instrument, its characterized in that: the device comprises a FP laser at the lower part and a metal array structure at the upper part, wherein a medium isolation layer is arranged on the light-emitting end face of the FP laser, a PDMS shell is arranged on the upper end face of the medium layer, the PDMS shell comprises a side wall and a top surface, a cavity formed by the side wall, the top surface and the upper end face of the medium layer is a micro-flow channel, a sample injection port and a sample outflow port are arranged on the top surface, and the sample injection port and the sample outflow port are positioned at two ends of the micro-flow; in the micro-flow channel, a metal array structure is arranged on the upper end face of the medium layer;
in the sensing detection of the sensing chip, a solution to be detected enters the sensing chip through a microfluidic channel of the PDMS shell, and the change of the light intensity of the FP laser before and after the solution to be detected is tested to realize chip sensing.
2. The FP laser-based sensor chip of claim 1, wherein: the dielectric isolation layer is a silicon dioxide layer or a silicon nitride layer.
3. The FP laser-based sensor chip of claim 1, wherein: the PDMS shell is a cylindrical structure with an opening at the bottom.
4. The FP laser-based sensor chip of claim 3, wherein: the PDMS shell is of a cuboid cylindrical structure.
5. The FP laser-based sensor chip of claim 1, wherein: the sensing chip based on the FP laser is arranged below the detector, and the top surface of the PDMS shell is opposite to the lower side of the detector.
6. The FP laser-based sensor chip of claim 1, wherein: the sample injection port and the sample outflow port are located at both ends of the top surface of the PDMS shell.
7. The method for preparing the sensor chip according to any one of claims 1 to 6, comprising the steps of:
(1) growing a film on the light emergent end face of the FP laser, wherein the film is a medium isolating layer;
(2) evaporating a layer of metal film on the medium isolation layer, and then manufacturing the metal film into a metal array structure by utilizing a micro-nano processing technology;
(3) a PDMS film with an opening at the bottom is manufactured by a PDMS mold turning technology to form a PDMS shell with a cylindrical structure;
(4) punching a hole at the top of the PDMS shell to form a sample injection port and a sample outflow port;
(5) and on the medium isolation layer, bonding the outer edges of the PDMS shell and the upper surface of the medium isolation layer after corona treatment to manufacture the sensing chip, wherein a cavity between the PDMS shell and the upper surface of the medium isolation layer is matched with the sample injection port and the sample outflow port to form a micro-flow channel.
8. The method according to claim 7, wherein: growing the dielectric film isolation layer in the step (1) by adopting a chemical vapor deposition or magnetron sputtering technology; the micro-nano processing technology in the step (2) adopts a focused ion beam direct writing technology or an electron beam exposure technology.
9. The method according to claim 7, wherein: and (5) treating the surfaces of the PDMS and the medium isolation layer by adopting a corona method to enable the two surfaces to form irreversible bonding so as to form a complete sensing chip.
10. The method according to claim 7, wherein: when the sensing chip is used for detecting specific molecules, a chemical modifier layer, a cross-linking agent layer and a biological monomolecular layer are added on the surface of the metal array structure; the chemical reagent used by the chemical modifier layer is dithiodiglycolic acid, the cross-linking agent layer is EDC/NHS, and the biomolecule layer is antigen, antibody, biotin, protein or nucleic acid molecule.
CN202011075860.3A 2020-10-10 2020-10-10 Sensing chip based on FP laser and metal array structure and preparation method thereof Pending CN112275333A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080105829A1 (en) * 2004-01-23 2008-05-08 Sri International Apparatus and Method of Moving Micro-Droplets Using Laser-Induced Thermal Gradients
CN104483498A (en) * 2014-12-24 2015-04-01 中国科学院半导体研究所 Sensing chip and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080105829A1 (en) * 2004-01-23 2008-05-08 Sri International Apparatus and Method of Moving Micro-Droplets Using Laser-Induced Thermal Gradients
CN104483498A (en) * 2014-12-24 2015-04-01 中国科学院半导体研究所 Sensing chip and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
崔小虹等: "《激光原理与技术实验》", 31 May 2017 *

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Application publication date: 20210129