CN110433878A - A kind of liquid detecting chip system of the optical phase difference based on VCSEL coupling array - Google Patents
A kind of liquid detecting chip system of the optical phase difference based on VCSEL coupling array Download PDFInfo
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- CN110433878A CN110433878A CN201910774171.2A CN201910774171A CN110433878A CN 110433878 A CN110433878 A CN 110433878A CN 201910774171 A CN201910774171 A CN 201910774171A CN 110433878 A CN110433878 A CN 110433878A
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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 kind of liquid detecting chip system of the optical phase difference based on VCSEL coupling array, belongs to the interleaving techniques field of semiconductor laser technology, biochemistry detection technology.The present invention induces the technologies such as anti-waveguide or photonic crystal by using H+implantation or chamber, realizes the preparation of VCSEL coupling array.By techniques such as PECVD, photoetching, sputtering, reactive ion etching, wet etching and bondings in VCSEL coupling array surface integrated micro-fluidic structure.Microflow control technique is utilized in VCSEL coupling array upper surface, testing liquid is passed through above VCSEL coupling array unit, light beam coupling phase difference between VCSEL unit is caused to change, so that laser beam deflects, by measuring laser beam deflection angle, the refractive index of liquid can be calculated, realizes liquid refractivity detection.
Description
Technical field
The invention belongs to the crossing domains of photoelectron technology and sensing technology, and in particular to one kind couples battle array based on VCSEL
The design of liquid refractivity sensing chip and preparation of column.
Background technique
Vertical cavity surface emitting laser (Vertical-cavity surface-emitting laser, VCSEL) has
The advantages that Low threshold, circular light spot, planar technology compatibility are easily integrated, has important in fields such as optic communication, optical interconnection, sensings
Using, and realize one of the perfect light source of micromation biochemical detection system (on piece laboratory).VCSEL coupling array is to pass through
Regulate and control the phase difference between array element, realizes the manipulation to laser beam, when laser array unit phase changes, wavefront
It can change, so that laser beam be made spatially to deflect.In VCSEL array coupling, by going out between change array element
The optical path difference for penetrating light may be implemented to regulate and control array element phase, to realize that light beam deflects.Based on this, it is proposed that a kind of
Liquid refractivity sensing chip based on VCSEL coupling array, using micro-fluidic on the basis of VCSEL coupling array planar structure
Testing liquid is passed through above VCSEL coupling array unit by technology, causes phase difference between VCSEL array element to change, so that laser light
Beam deflects, and by measuring laser beam deflection angle, can calculate the refractive index of liquid, realize liquid refractivity inspection
It surveys.Semiconductor laser technology and microflow control technique are combined by the sensing chip, have real-time, micro and detectable sample
The advantages such as range is wide.
Summary of the invention
Using VCSEL coupling array as laser light source, pass through the vapour deposition process (Plasma of plasma enhanced chemical
Enhanced chemical vapor deposition, PECVD), photoetching, sputtering, reactive ion etching (Reactive ion
Etching, RIE), the techniques such as wet etching and bonding integrate microchannel structure on VCSEL coupling array surface, complete chip
Preparation.Using microchannel structure, testing liquid is passed through above VCSEL coupling array unit, changes light beam between VCSEL unit
Coupled phase is poor, and laser beam is made to deflect, by calculating the refractive index of liquid to the measurement of laser beam deflection angle,
Realize liquid refractivity detection.
The present invention proposes a kind of liquid detecting chip system based on optical phase difference, solves the detection of traditional liquid refractive index
The problem of equipment, structure is complicated and is unable to real-time detection.Technical solution of the invention is as follows:
1. inducing the technologies such as anti-waveguide by H+implantation limitation or photonic crystal or chamber, make VCSEL array is each to shine
The light field of unit is coupled in device inside, has fixed phase relation between unit, so that high light beam quality can be obtained by preparing
The VCSEL coupling array of relevant light output;
2. integrating microchannel in VCSEL coupling array surface output optical zone by microflow control technique, inject testing liquid
Microchannel above above-mentioned specific VCSEL array unit, makes VCSEL array unit generate phase difference, deflects outgoing beam,
By measuring beam deflection angle, liquid refractivity is calculated.It the horizontal section schematic diagram of light beam sensing chip of the invention and bows
View difference is as depicted in figs. 1 and 2.
The preparation process of the sensing chip is as follows: then growth VCSEL epitaxial structure first uses H+implantation, light
Sub- crystal or chamber induce the technologies such as anti-waveguide, prepare VCSEL by techniques such as PECVD, photoetching, sputtering, etching, H+implantations
Coupling array, to obtain coherent laser output;Two sides production Ti/Au in VCSEL epitaxial structure upper surface separates electrode, In
Bottom surface prepares AuGeNi/Au rear electrode, is annealed with quick anneal oven to resulting structures, makes electrode and epitaxial wafer surface shape
At good Ohmic contact;Then use PECVD in VCSEL array surface growth thickness for the SiO of 3~10 μ m-thicks2Layer;With gold
Belong to Ni and do exposure mask, using RIE technique by the SiO above VCSEL array unit output optical zone2It etches away, is formed as shown in FIG. 6
Microchannel, while retaining the SiO of 500nm in the bottom of microchannel2Prevent VCSEL cell electrode from leaking electricity;By poly dimethyl
Silicone compositions (PDMS) are stood in culture dish on silicon wafer, and the thickness of PDMS is about 3mm, the baking for being 70-80 DEG C in temperature
It is dried 30 minutes on platform, makes the solid PDMS film with a thickness of 3mm;Two injecting fluids are outputed in PDMS film surface with punch
Hole;PDMS is bonded to facet surface, in the production for completing chip.
The VCSEL coupling array includes that H+implantation coupling array, photon crystal coupled array and chamber induction are anti-
Waveguide coupling array etc. can obtain the VCSEL array of relevant light output.
The coupling array laser source surface VCSEL be equipped with M × N number of VCSEL unit, M, N at least one be greater than etc.
In 2.
The top of each VCSEL unit output optical zone corresponds to a microchannel, and microchannel is in VCSEL unit output optical zone
The position of top cover corresponding output optical zone;Passage portion width of each microchannel in output optical zone two sides is opposite to become larger.
The VCSEL coupling array laser source makes each VCSEL array element have independent electricity using separation electrode design
The independent control to each array element is realized in pole.
The material of the microchannel is not limited to PDMS, can be any material for being able to achieve microchannel.
It has the beneficial effect that brought by the present invention: using VCSEL coupling array as laser source, being increased by plasma
The vapour deposition process (Plasma enhanced chemical vapor deposition, PECVD) of extensive chemical, splashes at photoetching
Penetrate, the techniques such as reactive ion etching (Reactive ion etching, RIE), wet etching and bonding integrated on its surface it is micro-
The micro-fluidic module such as circulation road injects testing liquid above specific VCSEL array unit, and VCSEL array element is made to generate phase
Difference causes light beam to deflect, and by measuring beam deflection angle, calculates liquid refractivity.The sensing chip is by semiconductor laser
Technology is combined with microflow control technique, has the advantages such as real-time, micro and detectable sample scope is wide.VCSEL coupling array
It is capable of providing uniformly relevant light output, it can by conventional semiconducter process using its planar technology compatibility characteristic
Microchannel structure is easily integrated into its surface, completes the preparation of sensing chip, which has small in size, real-time inspection
It surveys, the advantages such as trace detection and detection range are wide, is had a good application prospect in biochemistry detection field.
Detailed description of the invention
Fig. 1: the sectional view of sensing chip;
Fig. 2: the top view of sensing chip;
The structural schematic diagram of Fig. 3: VCSEL coupling array;
Fig. 4: 2 μm or more of SiO is grown on VCSEL array surface using PECVD2Structural schematic diagram afterwards;
Fig. 5: sputtering and removes, and makes the structural schematic diagram of W metal exposure mask;
Fig. 6: Ni, which does exposure mask, etches SiO using RIE technique2, make the structural schematic diagram of microchannel;
Fig. 7: wet etching removes Ni, and in SiO2Surface bond PDMS completes the structural schematic diagram of chip preparation;
In figure: 1, VCSEL epitaxial wafer substrate, 2, N-type DBR, 3, active area, 4, p-type DBR, 5, SiO2, 6, Ni, 7, proton
Injection region, 8, Ti/Au positive electrode, 9, back side AuGeNi/Au negative electrode, 10, PDMS plate face, 11 microchannel areas, 12, VCSEL
Array element.
Specific embodiment
Embodiment 1
By taking the integrated micro-fluidic of H+implantation type VCSEL coupling array surface as an example, of the invention is described in detail.
VCSEL coupling array is introduced respectively below with reference to Fig. 3-Fig. 7 to pass with the liquid refractivity that microchannel on piece integrates
The specific embodiment of the preparation method of sense chip;
Step 1, using metal organic chemical vapor deposition (MOCVD) on N-GaAs successively 34 pairs of epitaxial growth
n-Al(0.12-0.9)GaAs and n-Al0.9GaAs constitutes DBR reflecting mirror, Al(0.12-0.9)GaAs/Al0.9GaAs lower limit layer, three pairs
Al0.3GaAs/GaAs quantum well structure active area, Al0.9GaAs/Al(0.12-0.9)GaAs upper limiting layer, 22.5 couples of p-Al0.12GaAs
With p-Al(0.9-0.12)GaAs constitutes DBR reflecting mirror, p-Al0.12GaAs and p-GaAs heavy doping contact layer;
Step 2 grows one on epitaxial wafer surface obtained above using plasma enhanced CVD (PECVD)
The silica of 3.5 μm of layer;
Step 3, using photoetching and sputtering technology, prepare with a thickness of 300nm W metal exposure mask;
Step 4 removes light hole (the distance between light hole using sense coupling method (RIE) etching
It is 4 microns, is the array of 2X1) silica in other regions outside, etch thicknesses are 3 μm, and remaining 0.5 μm prevents H+implantation
When generate channelling effect and control H+implantation depth, to complete the production of H+implantation exposure mask;
Step 5 carries out H in obtained above son using H+implantation method+Injection, first time Implantation Energy are
315keV, second of Implantation Energy is 250keV, and implantation dosage is 1E15cm twice-2;
Step 6 is protected using photoresist to board marker, with the silica on wet etching method removal epitaxial wafer surface;
Step 7, using reversion glue do photoetching and sputtering technology right above injection region surface sputtering with a thickness ofTi/Au peripheral electrode, peel off the metal in light hole region in conjunction with ultrasound with acetone, that is, remove light hole
Region without Ti/Au outside, other regions are all covered with Ti/Au;
Step 8, sputteringAuGeNi/Au rear electrode;
Step 9 makes piece form good Ohmic contact using rapid thermal annealing (350 degrees Celsius, annealing time 35s),
Complete the preparation of VCSEL coupling array;
Step 10 grows one layer 6 μm of SiO on VCSEL coupling array obtained above surface using PECVD2, utilizeNickel does exposure mask, etches fluid passage with RIE, etch thicknesses are 5.5 μm;
Step 11 is put into sizable clean silicon wafer bottom in culture dish, and PDMS material is poured into culture dish,
The thickness of PDMS is about 3mm, is stood, be to dry 30 minutes on 70-80 DEG C of baking platform in temperature, we have obtained thickness in this way
For the solid PDMS film of 3mm;
Step 12, cutting out the rectangular type PDMS film of 0.8cm × 1cm, (0.8cm is to expose and make epitaxial wafer edge
VCSEL array electrode is convenient for pressure welding), and finally should with punch in the hole got for liquid injection on the surface PDMS
PDMS is bonded with VCSEL coupling array;
Steel needle is inserted into PDMS liquid injection hole, and connects syringe pump with hose by step 13, is infused liquid with syringe pump
Enter microchannel.
It is obtained using FDTD theoretical calculation, the deflection angle of water and dehydrated alcohol is 1.03 ° and 1.95 ° respectively.To chip
Microchannel in injection be injected separately into water and dehydrated alcohol, the beam deflection angle tested is respectively 1.08 ° and 1.70 °,
Experimental error is that the faulty coherence of VCSEL coupling array is caused to cause due to defective workmanship, to further be reflected
Rate.
The foregoing is merely better embodiments of the invention, are not intended to limit the invention, all in design of the invention
Any modification, replacement and improvement etc. with making under the premise of design, are considered as being included within protection scope of the present invention.
Claims (8)
1. a kind of liquid detecting chip system of the optical phase difference based on VCSEL coupling array, it is characterised in that:
S1. anti-guide technology is induced by H+implantation limitation or photonic crystal or chamber, makes each luminescence unit of VCSEL array
Light field coupled in device inside, have fixed phase relation between unit, can to obtain high light beam quality relevant to prepare
The VCSEL coupling array of light output;
S2. microchannel is integrated in VCSEL coupling array surface output optical zone by microflow control technique, keeps testing liquid injection above-mentioned
Microchannel above specific VCSEL array unit, makes VCSEL array unit member generate phase difference, deflects outgoing beam, leads to
Measuring beam deflection angle is crossed, liquid refractivity is calculated.
2. a kind of liquid detecting chip system of optical phase difference based on VCSEL coupling array described in accordance with the claim 1,
It is characterized by:
The VCSEL coupling array includes that H+implantation coupling array, photon crystal coupled array and chamber induce anti-waveguide
Coupling array etc. can obtain the VCSEL array of relevant light output.
3. a kind of liquid detecting chip system of optical phase difference based on VCSEL coupling array described in accordance with the claim 1,
It is characterized by: the coupling array laser source surface VCSEL is equipped with M × N number of VCSEL unit, M, N at least one are greater than
Equal to 2.
4. a kind of liquid detecting chip system of optical phase difference based on VCSEL coupling array described in accordance with the claim 1,
It is characterized by: the top of each VCSEL unit output optical zone corresponds to a microchannel, microchannel goes out in VCSEL unit
The position of the top in light area covers corresponding output optical zone;Passage portion width of each microchannel in output optical zone two sides is opposite to be become
Greatly.
5. a kind of liquid detecting chip system of optical phase difference based on VCSEL coupling array described in accordance with the claim 1,
It is characterized by: the VCSEL coupling array laser source has each VCSEL array element independent using separation electrode design
Electrode realizes the independent control to each array element.
6. a kind of liquid detecting chip system of optical phase difference based on VCSEL coupling array according to claim 1
Preparation process, it is characterised in that: first growth VCSEL epitaxial structure, then using H+implantation, photonic crystal or chamber induction
The technologies such as anti-waveguide prepare VCSEL coupling array by techniques such as photoetching, sputtering, PECVD, etching, H+implantations, to obtain
Must be concerned with light output;Utilize photoetching and sputtering technology, preparative separation electrode;Then using PECVD in VCSEL array surface deposition
A layer thickness is the SiO of 3~10 μ m-thicks2Or SiNx;Ni does the method for exposure mask RIE etching in SiO2Or SiNxUpper quarter miniflow is logical
Road;PDMS material is stood in culture dish on silicon wafer, the thickness of PDMS is about 3mm, on the baking platform that temperature is 70-90 DEG C
It dries 30 minutes, makes the solid PDME film with a thickness of 3mm;It is beaten with punch and outputs two injecting fluids on the surface PDMS
Hole;PDMS is bonded to facet surface;It is inserted into steel needle in the injection orifice of PDMS and injects liquid into miniflow with syringe pump and leads to
In road, in the production for completing chip.
7. preparation process according to claim 6, it is characterised in that: the material of the microchannel is not limited to PDMS,
It can be any material for being able to achieve microchannel.
8. preparation process according to claim 6, it is characterised in that: specific steps include the following:
Step 1, using metal organic chemical vapor deposition (MOCVD) on N-GaAs successively 34 couples of n- of epitaxial growth
Al(0.12-0.9)GaAs and n-Al0.9GaAs constitutes DBR reflecting mirror, Al(0.12-0.9)GaAs/Al0.9GaAs lower limit layer, three pairs
Al0.3GaAs/GaAs quantum well structure active area, Al0.9GaAs/Al(0.12-0.9)GaAs upper limiting layer, 22.5 couples of p-Al0.12GaAs
With p-Al(0.9-0.12)GaAs constitutes DBR reflecting mirror, p-Al0.12GaAs and p-GaAs heavy doping contact layer;
Step 2 grows one layer on epitaxial wafer surface obtained above using plasma enhanced CVD (PECVD)
3.5 μm of silica;
Step 3, using photoetching and sputtering technology, prepare with a thickness of 300nm W metal exposure mask;
Step 4, the silica that other regions in addition to light hole are etched using sense coupling method (RIE),
Etch thicknesses are 3 μm, and remaining 0.5 μm prevents from generating channelling effect and control H+implantation depth when H+implantation, to complete
The production of H+implantation exposure mask;
Step 5 carries out H in obtained above son using H+implantation method+Injection, first time Implantation Energy are 315keV, the
Secondary Implantation Energy is 250keV, and implantation dosage is 1E15cm twice-2;
Step 6 is protected using photoresist to board marker, with the silica on wet etching method removal epitaxial wafer surface;
Step 7, using reversion glue do photoetching and sputtering technology right above injection region surface sputtering with a thickness of
Ti/Au peripheral electrode, peel off the metal in light hole region in conjunction with ultrasound with acetone, i.e., in addition to light hole region is without Ti/Au,
Other regions are all covered with Ti/Au;
Step 8, sputteringAuGeNi/Au rear electrode;
Step 9 makes piece form good Ohmic contact using rapid thermal annealing, completes the preparation of VCSEL coupling array;
Step 10 grows one layer 6 μm of SiO on VCSEL coupling array obtained above surface using PECVD2, utilize
Nickel does exposure mask, etches fluid passage with RIE, etch thicknesses are 5.5 μm;
Step 11 is put into sizable clean silicon wafer bottom in culture dish, and PDMS material is poured into culture dish, PDMS's
Thickness is about 3mm, is stood, be to dry 30 minutes on 70-80 DEG C of baking platform in temperature, we have obtained with a thickness of 3mm in this way
Solid PDMS film;
Step 12, cutting out the rectangular type PDMS of 0.8cm × 1cm, (0.8cm is to expose the VCSEL array for making epitaxial wafer edge
Electrode is convenient for pressure welding), and with punch in the hole got for liquid injection on the surface PDMS, finally by the PDMS and VCSEL
Coupling array is bonded;
Steel needle is inserted into PDMS liquid injection hole, and connects syringe pump with hose by step 13, is injected liquid into syringe pump micro-
Circulation road.
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