CN110433878B - Liquid detection chip based on VCSEL coupling array optical phase difference - Google Patents
Liquid detection chip based on VCSEL coupling array optical phase difference Download PDFInfo
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- CN110433878B CN110433878B CN201910774171.2A CN201910774171A CN110433878B CN 110433878 B CN110433878 B CN 110433878B CN 201910774171 A CN201910774171 A CN 201910774171A CN 110433878 B CN110433878 B CN 110433878B
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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
- 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
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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
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
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- 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
- H01S5/00—Semiconductor lasers
- H01S5/10—Construction or shape of the optical resonator, e.g. extended or external cavity, coupled cavities, bent-guide, varying width, thickness or composition of the active region
- H01S5/18—Surface-emitting [SE] lasers, e.g. having both horizontal and vertical cavities
- H01S5/183—Surface-emitting [SE] lasers, e.g. having both horizontal and vertical cavities having only vertical cavities, e.g. vertical cavity surface-emitting lasers [VCSEL]
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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
- B01L2300/00—Additional constructional details
- B01L2300/08—Geometry, shape and general structure
- B01L2300/0809—Geometry, shape and general structure rectangular shaped
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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
- B01L2300/00—Additional constructional details
- B01L2300/08—Geometry, shape and general structure
- B01L2300/0887—Laminated structure
Abstract
A liquid detection chip system based on VCSEL coupling array optical phase difference belongs to the cross technical field of semiconductor laser technology and biochemical detection technology. The invention realizes the preparation of the VCSEL coupling array by adopting the technologies of proton injection, cavity induced inverse waveguide, photonic crystal and the like. And integrating the microfluidic structure on the surface of the VCSEL coupling array by processes of PECVD, photoetching, sputtering, reactive ion etching, wet etching, bonding and the like. The micro-fluidic technology is utilized on the upper surface of the VCSEL coupling array, liquid to be detected is introduced above the VCSEL coupling array units, light beam coupling phase difference among the VCSEL units is changed, laser beams are deflected, the refractive index of the liquid can be calculated by measuring the deflection angle of the laser beams, and liquid refractive index detection is achieved.
Description
Technical Field
The invention belongs to the crossing field of photoelectron technology and sensing technology, and particularly relates to design and preparation of a liquid refractive index sensing chip based on a VCSEL (vertical cavity surface emitting laser) coupling array.
Background
A Vertical-cavity surface-emitting laser (VCSEL) has the advantages of low threshold, circular light spot, compatible planar process, easy integration and the like, has important application in the fields of optical communication, optical interconnection, sensing and the like, and is also one of ideal light sources for realizing a miniaturized detection system (lab-on-a-chip). The VCSEL coupling array controls laser beams by regulating and controlling phase differences among array elements, and when the phases of laser array units are changed, the wave fronts of the laser array units can be changed, so that the laser beams are deflected in space. In VCSEL array coupling, the phase of an array unit can be regulated and controlled by changing the optical path difference of emergent light among array elements, so that light beam deflection is realized. Based on the liquid refractive index sensing chip based on the VCSEL coupling array, a microfluidic technology is utilized on the basis of a VCSEL coupling array plane structure, liquid to be detected is introduced above the VCSEL coupling array unit, phase difference among VCSEL array elements is changed, laser beams are deflected, the refractive index of the liquid can be calculated through measuring the deflection angle of the laser beams, and liquid refractive index detection is achieved. The sensing chip combines the semiconductor laser technology with the microfluidic technology, and has the advantages of real time, trace quantity, wide detectable sample range and the like.
Disclosure of Invention
The preparation method comprises the steps of adopting a VCSEL coupling array as a laser light source, and integrating a microfluidic channel structure on the surface of the VCSEL coupling array through Plasma Enhanced Chemical Vapor Deposition (PECVD), photoetching, sputtering, Reactive Ion Etching (RIE), wet etching, bonding and other processes to finish the preparation of a chip. The liquid to be detected is introduced above the VCSEL coupling array unit by utilizing the micro-flow channel structure, the light beam coupling phase difference among the VCSEL units is changed, the laser beam is deflected, the refractive index of the liquid is calculated by measuring the deflection angle of the laser beam, and the detection of the refractive index of the liquid is realized.
The invention provides a liquid detection chip based on optical phase difference, which solves the problems that the traditional liquid refractive index detection equipment is complex in structure and cannot detect in real time. The technical solution of the invention is as follows:
1. the light fields of all light emitting units of the VCSEL array are coupled in the device through proton injection limitation or photonic crystals or cavity induced inverse waveguide and other technologies, and a fixed phase relationship exists among the units, so that the VCSEL coupled array capable of obtaining high-beam-quality coherent light output is prepared;
2. a microfluidic channel is integrated on a light-emitting area on the surface of the VCSEL coupling array through a microfluidic technology, so that liquid to be detected is injected into the microfluidic channel above the specific VCSEL array unit, the VCSEL array unit generates phase difference, an emergent light beam is deflected, and the refractive index of the liquid is calculated through measuring the deflection angle of the light beam. The schematic diagram of the transverse section and the top view of the light beam sensing chip of the present invention are shown in fig. 1 and fig. 2, respectively.
The preparation process of the sensing chip comprises the following steps: firstly growing a VCSEL epitaxial structure, and then preparing a VCSEL coupling array by adopting the technologies of proton injection, photonic crystal or cavity induced inverse waveguide and the like through the processes of PECVD, photoetching, sputtering, etching, proton injection and the like so as to obtain coherent laser output; manufacturing Ti/Au separation electrodes on two side edges of the upper surface of the VCSEL epitaxial structure, preparing an AuGeNi/Au back electrode on the bottom surface, and annealing the obtained structure by using a rapid annealing furnace to form good ohmic contact between the electrodes and the surface of an epitaxial wafer; then, growing SiO with the thickness of 3-10 μm on the surface of the VCSEL array by adopting PECVD2A layer; using metal Ni as a mask, and using RIE (reactive ion etching) process to remove SiO above the light emergent area of the VCSEL array unit2Etching away to form the microfluidic channel shown in FIG. 6, while keeping 500nm of SiO at the bottom of the microfluidic channel2Preventing leakage of the VCSEL unit electrodes; standing Polydimethylsiloxane (PDMS) material in a culture dish on a silicon chip, wherein the thickness of the PDMS is about 3mm, and baking the PDMS material on a baking table at the temperature of 70-80 ℃ for 30 minutes to manufacture a solid PDMS membrane with the thickness of 3 mm; using a puncher to open two holes for injecting liquid on the surface of the PDMS membrane; and bonding PDMS to the surface of the laser to complete the manufacture of the chip.
The VCSEL coupling array comprises a proton injection coupling array, a photonic crystal coupling array, a cavity induced inverse waveguide coupling array and the like, and the VCSEL array can obtain coherent light output.
The surface of the VCSEL coupling array laser source is provided with M multiplied by N VCSEL units, and at least one of M and N is more than or equal to 2.
The upper part of each VCSEL unit light-emitting area corresponds to a microfluidic channel, and the microfluidic channel covers the corresponding light-emitting area at the position above the light-emitting area of the VCSEL unit; the width of partial channels of each micro-flow channel on two sides of the light emergent area is relatively larger.
The VCSEL coupled array laser source adopts a separated electrode design, so that each VCSEL array element has an independent electrode, and the independent control of each array element is realized.
The material of the microfluidic channel is not limited to PDMS, and may be any material that can realize the microfluidic channel.
The beneficial effects brought by the invention are as follows: a VCSEL coupling array is used as a laser source, microfluidic modules such as microfluidic channels are integrated on the surface of the VCSEL coupling array through Plasma Enhanced Chemical Vapor Deposition (PECVD), photoetching, sputtering, Reactive Ion Etching (RIE), wet etching, bonding and other processes, liquid to be detected is injected above a specific VCSEL array unit, the VCSEL array unit generates phase difference to cause light beam deflection, and the refractive index of the liquid is calculated through measuring the light beam deflection angle. The sensing chip combines the semiconductor laser technology with the microfluidic technology, and has the advantages of real time, trace quantity, wide detectable sample range and the like. The VCSEL coupling array can provide uniform coherent light output, and the microfluidic channel structure can be easily integrated on the surface of the VCSEL coupling array by utilizing the characteristic of plane process compatibility of the VCSEL coupling array through a conventional semiconductor processing process to complete the preparation of a sensing chip.
Drawings
FIG. 1: a cross-sectional view of the sensor chip;
FIG. 2: a top view of the sensing chip;
FIG. 3: the structure of the VCSEL coupling array is schematic;
FIG. 4: growing SiO with the diameter of more than 2 mu m on the surface of the VCSEL array by utilizing PECVD2A rear structure schematic diagram;
FIG. 5: sputtering and stripping to manufacture a structural schematic diagram of a metal Ni mask;
FIG. 6: etching SiO by RIE process using Ni as mask2Making a structural schematic diagram of the microfluidic channel;
FIG. 7: wet etching to remove Ni and form SiO2Bonding PDMS on the surface to finish the structural schematic diagram of chip preparation;
in the figure: 1. VCSEL epitaxial wafer substrate, 2, N-type DBR, 3, active region, 4, P-type DBR, 5, SiO 26, Ni, 7, a proton injection area, 8, a Ti/Au positive electrode, 9, a back AuGeNi/Au negative electrode, 10, a PDMS plate surface, 11 a micro-flow channel area, 12 and a VCSEL array unit.
Detailed Description
Example 1
The present invention will be described in detail by taking the proton injection type VCSEL coupled array surface integrated microfluidics as an example.
The following describes embodiments of the method for manufacturing the VCSEL coupling array and the liquid refractive index sensor chip integrated on the microchannel plate with reference to fig. 3 to 7;
and step 13, inserting a steel needle into the PDMS liquid injection hole, connecting a syringe pump with a hose, and injecting the liquid into the microfluidic channel with the syringe pump.
The deflection angles of water and absolute ethyl alcohol were 1.03 ° and 1.95 °, respectively, as calculated using the FDTD theory. Water and absolute ethyl alcohol are respectively injected into a microfluidic channel of the chip, the light beam deflection angles obtained by testing are respectively 1.08 degrees and 1.70 degrees, experimental errors are caused by imperfect coherence of a VCSEL coupling array due to process defects, and therefore the refractive index is further obtained.
The above description is only a preferred embodiment of the present invention and should not be taken as limiting the invention, and any modifications, substitutions, improvements and the like made on the premise of the design and concept of the present invention should be considered to be included in the protection scope of the present invention.
Claims (7)
1. A liquid detection chip based on optical phase difference of VCSEL coupling array is characterized in that:
s1, coupling optical fields of all light emitting units of a VCSEL array in a device through proton injection limitation and photonic crystal or cavity induced inverse waveguide technology, wherein the units have a fixed phase relation, so that the VCSEL coupled array capable of obtaining high-beam-quality coherent light output is prepared;
s2, integrating a microfluidic channel in a light emergent area on the surface of the VCSEL coupling array through a microfluidic technology; when liquid to be measured is injected into a microfluidic channel on the surface of the VCSEL coupling array, phase difference can be generated among the VCSEL coupling array units, outgoing light beams are deflected, and the refractive index of the liquid is calculated by measuring the deflection angle of the light beams.
2. The VCSEL coupling array based liquid detection chip system with optical phase difference according to claim 1, wherein:
the VCSEL coupling array comprises a proton injection coupling array, a photonic crystal coupling array and a cavity-induced inverse waveguide coupling array, and the VCSEL coupling array can obtain coherent light output.
3. The VCSEL coupling array based liquid detection chip system with optical phase difference according to claim 1, wherein: the number of the VCSEL coupling array units is M multiplied by N, wherein at least one of M and N is more than or equal to 2.
4. The VCSEL coupling array based liquid detection chip system with optical phase difference according to claim 1, wherein: two or more micro-channels can be prepared above the VCSEL coupling array unit; one of the micro-channels is used as a liquid detection channel, and the other micro-channels are used as refractive index filling channels; by injecting liquid with known refractive index into the refractive index filling channel, the refractive index range of the liquid detected by the chip can be expanded.
5. The VCSEL coupling array based liquid detection chip system with optical phase difference according to claim 1, wherein: the VCSEL coupled array laser source adopts a separated electrode design, so that each VCSEL array element has an independent electrode, and independent current control is realized on each array unit of the VCSEL coupled array.
6. The process of claim 1, wherein the liquid detection chip comprises a liquid crystal layer and a liquid crystal layer, wherein the liquid crystal layer comprises a plurality of optical phase differences, and the optical phase differences comprise optical phase differences of VCSEL coupled arrays, wherein the optical phase differences comprise: firstly growing a VCSEL epitaxial structure, and then preparing a VCSEL coupling array by adopting a proton injection technology, a photonic crystal technology or a cavity induced inverse waveguide technology through photoetching, sputtering, PECVD, etching and proton injection technologies so as to obtain coherent light output; preparing a separation electrode by utilizing photoetching and sputtering processes; then, a layer of SiO with the thickness of 3-10 mu m is deposited on the surface of the VCSEL array by adopting PECVD2Or SiNx(ii) a RIE etching method using Ni as mask on SiO2Or SiNxA microfluidic channel is formed; placing PDMS material in a culture dish on a silicon chip, wherein the thickness of PDMS is 3mm, and the temperature is 7 DEGBaking for 30 minutes on a baking table at the temperature of 0-90 ℃ to prepare a solid PDMS film with the thickness of 3 mm; punching two holes for injecting liquid on the surface of PDMS by using a puncher; bonding PDMS to a laser surface; and inserting a steel needle into the injection hole of the PDMS, injecting liquid into the microfluidic channel by using an injection pump, and finishing the manufacture of the chip.
7. The process according to claim 6, characterized in that: the method comprises the following specific steps:
step 1, sequentially epitaxially growing thirty-four pairs of N-Al on N-GaAs by adopting metal organic chemical vapor deposition(0.12-0.9)GaAs with n-Al0.9GaAs forms a DBR mirror, Al(0.12-0.9)GaAs/Al0.9Lower confinement layer of GaAs, three pairs of Al0.3GaAs/GaAs Quantum well Structure active region, Al0.9GaAs/Al(0.12-0.9)Upper confinement layer of GaAs, 22.5 p-Al0.12GaAs with p-Al(0.9-0.12)GaAs form a DBR mirror, p-Al0.12GaAs and p-GaAs are heavily doped to contact the layer, finish the growth of VCSEL epitaxial wafer;
step 2, growing a layer of silicon dioxide with the thickness of 3.5 microns on the surface of the epitaxial wafer prepared in the step 1 by utilizing a plasma enhanced chemical vapor deposition technology;
step 3, preparing a metal Ni mask with the thickness of 300nm by utilizing photoetching and sputtering processes;
step 4, etching the silicon dioxide in other areas except the light outlet hole by using an inductive coupling plasma etching method, wherein the etching thickness is 3 microns, and the remaining 0.5 micron prevents a channel effect from being generated during proton implantation and controls the proton implantation depth, thereby completing the manufacture of a proton implantation mask;
step 5, performing H in the sample obtained in the step 4 by proton implantation+Implanting at 315keV for the first time and 250keV for the second time, wherein the two implantations are performed at a dose of 1E15cm-2；
Step 6, protecting the register mark by using photoresist, and removing silicon dioxide on the surface of the epitaxial wafer by using a wet etching method;
step 7, using the reverse photoresist to carry out photoetching and sputtering processes on the surface right above the injection regionSputtering to a thickness of
The Ti/Au peripheral electrode strips the metal of the light hole area by combining acetone and ultrasound, namely, the Ti/Au is covered on other areas except the light hole area without the Ti/Au;
step 8, sputtering
The AuGeNi/Au back electrode of (1);
9, forming good ohmic contact on the wafer by utilizing rapid thermal annealing to finish the preparation of the VCSEL coupling array;
step 10, growing a layer of SiO with the thickness of 6 microns on the surface of the VCSEL coupling array obtained by the method through PECVD2By using
Nickel is used as a mask, RIE is used for etching a liquid channel, and the etching thickness is 5.5 mu m;
step 11, placing the bottom of a clean silicon wafer with the same size in a culture dish, pouring a PDMS material into the culture dish, standing, and baking for 30 minutes on a baking table at the temperature of 70-80 ℃ to obtain a solid PDMS membrane with the thickness of 3 mm;
12, cutting out 0.8cm × 1cm square PDMS, punching a hole for liquid injection on the surface of the PDMS by using a puncher, and finally bonding the PDMS with the VCSEL coupling array;
and step 13, inserting a steel needle into the PDMS liquid injection hole, connecting a syringe pump with a hose, and injecting the liquid into the microfluidic channel with the syringe pump.
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| CN114268020B (en) * | 2021-11-16 | 2023-11-28 | 深圳市嘉敏利光电有限公司 | Al with high refractive index contrast 2 O 3 Al x Ga 1-x As DBR VCSEL manufacturing method |
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