CN109596572A - A kind of gas sensor and preparation method thereof - Google Patents
A kind of gas sensor and preparation method thereof Download PDFInfo
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- CN109596572A CN109596572A CN201811547367.XA CN201811547367A CN109596572A CN 109596572 A CN109596572 A CN 109596572A CN 201811547367 A CN201811547367 A CN 201811547367A CN 109596572 A CN109596572 A CN 109596572A
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Abstract
The invention discloses a kind of gas sensors, including substrate and the gain media layer being deposited on substrate；Substrate surface has ring-shaped groove.The invention also discloses a kind of gas sensor preparation methods, specifically include following step: using lithographic etch process in quartz glass substrate surface processing ring-shaped groove as gas sensor main body；The quantum dot that deposited polymer adulterates in gas sensor main body completes the gas sensor production based on piece quantum dot microcavity as gain media layer.The transmission mechanism testing gas concentration that the present invention causes excitation wavelength mobile using gain media deformation and variations in refractive index, test macro is simple, and Yi Shixian on piece is integrated, is miniaturized, and portability is strong.
Description
Technical field
The invention belongs to gas concentration measurement technical fields, in particular to a kind of to be based on polymer-doped type quantum dot optics
Gas sensor of microcavity and preparation method thereof.
Background technique
In actual life, light concentration gas detection is most important in numerous occasions.For example, in the enforcing law of drunk driving,
In environment monitoring poisonous gas, in hazardous gas constituent analysis and in flammable explosive gas manufacture transportational process, gas content
How much direct relation people's normal lifves order and health.The gas componant for how efficiently detecting low concentration becomes sensing
Device research field is worth the project of development.
Gas sensor belongs to one kind of chemical sensor, specifically includes that semiconductor gas sensor, electrochemical gas pass
Sensor, catalytic combustion method gas sensor, thermal conductivity gas sensor, infrared gas sensor, solid-electrolyte gas pass
Sensor etc..In the gas sensor of numerous types, majority of gas sensor all use biochemistry, electrochemistry, physics and
Optical design principle.Wherein, optical gas sensor is because electromagnetism interference is strong, and fast response time, recovery time is short, spirit
The advantages such as sensitivity is high, easy of integration, and size is small are in recent years by the concern of researcher.
For different test gas, in order to improve the sensitivity of detection of gas, researcher has selected different absorptions
Material and transmission mechanism, such as metal oxide, polymer, carbon allotrope, quantum cascade laser, overarm arm and
Narrow slit wave-guide etc..Therefore, different types of detection of gas transmission mechanism is explored, the optical material of different sensitivity is selected, it is right
The type for further expanding gas sensor enhances its detection of gas sensitivity with positive facilitation.
Summary of the invention
The shortcomings that it is a primary object of the present invention to overcome the prior art and insufficient, provides a kind of gas sensor and its system
Preparation Method, the transmission mechanism testing gas concentration for causing excitation wavelength mobile using gain media deformation and variations in refractive index,
Its test macro is simple, and Yi Shixian on piece is integrated, is miniaturized, and portability is strong.
The purpose of the present invention is realized by the following technical solution: a kind of gas sensor, including substrate and is deposited on base
The gain media layer of on piece；Substrate surface has ring-shaped groove.
Preferably, the substrate is quartz glass substrate, and with a thickness of 5um-4mm, it is 0.1um- that ring-shaped groove, which etches width,
500um, etching depth 0.1um-500um.
Preferably, the gain media layer includes Colloidal Quantum Dots layer and cured polymeric layer thereon, gain media layer
Thickness between 0.1um-500um.
Further, the Colloidal Quantum Dots layer is the monokaryon quantum dot of binary or ternary or quaternary, or for binary or
The core-shell type quantum point of ternary or quaternary, or be the quantum dot gain material after surface hydroxylation or amination functionalized modification；Amount
The concentration of son point is 1mg/mL-100mg/mL.
Further, the polymer be polystyrene PS or polymetylmethacrylate or polycarbonate or
Common thermoplastics type's light functional polymer material such as COC；Polymer-doped mass fraction is 0.1%-10%.
Preferably, the gain media layer is that polymer-doped quantum dot layer or organic dye layer or organic dyestuff are compound
Nitride layer or rare earth ion layer or rare earth ion composite layer or semiconducting organic polymer layer or pure quantum dot layer or quantum dot are multiple
Close nitride layer；By depositing different types of gain media, the selectivity of gas with various detection target may be implemented.
A kind of gas sensor preparation method, specifically includes following step:
S1, ring-shaped groove is processed as gas sensor main body on quartz glass substrate surface using lithographic etch process；
S2, the quantum dot that deposited polymer adulterates in gas sensor main body are completed to be based on piece as gain media layer
The gas sensor of upper quantum dot microcavity makes.
Preferably, the step S1 selects the quartz glass substrate smooth with a thickness of 5um-4mm, surface, using partly leading
The method of body chemical wet etching processes ring-shaped groove on quartz glass substrate surface.
Further, for the chemical wet etching of quartz glass substrate on piece ring-shaped groove, ring-shaped groove in the step S1
Etching width be 0.1um-500um, etching depth 0.1um-500um；It etches coil power and is lower than 2000W, radio-frequency power
Lower than 1000W, etching gas C4F8Flow velocity is lower than 100sccm, and He flow velocity is lower than 30sccm.
Preferably, the work of the step S2 quantum dot gain medium that deposited polymer adulterates in gas sensor main body
Skill step are as follows: mix a certain amount of polymer and Colloidal Quantum Dots solution first, it is desirable that mixed solution is evenly distributed, and does not sink
It forms sediment, gain medium material is deposited using the method for spin coating later, the gas sensing based on quantum dot microcavity can be completed after solidification
Device prototype.
Further, the step S2 is selected as polystyrene PS or polymetylmethacrylate to polymer
Or common thermoplastics type's light functional polymer material such as polycarbonate or COC；Meanwhile polymer-doped mass fraction is
0.1%-10%.
Further, Colloidal Quantum Dots layer choosing selects the monokaryon quantum dot of binary or ternary or quaternary in the step S2,
Such as CdSe, CdTe, CdSeS etc., or the core-shell type quantum point of selection binary or ternary or quaternary, such as CdSe/ZnS,
Special quantum dot gain material after CdSeS/ZnS isocolloid quantum dot, or the selection functionalized modifications such as surface hydroxylation or amination
Material；Meanwhile the concentration of quantum dot is controlled in 1mg/mL-100mg/mL.
Further, the thickness for the quantum dot gain medium that deposited polymer adulterates in the step S2 is in 0.1um-
Between 500um, and polymer-doped quantum dot gain medium has good conformality in ring-shaped groove side wall.
Preferably, the gas sensor preparation method after removing cured gain material layer, can deposit gain Jie again
Matter.
Preferably, the gain media selects pure quantum dot or quantum dot compound or organic dyestuff or organic dyestuff compound
Object or rare earth ion or the common gain media such as rare earth ion compound or semiconducting organic polymer.By depositing inhomogeneity
The selectivity of gas with various detection target may be implemented in the gain media of type.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1, the present invention is using the polymer-doped type quantum dot gain medium layer combination high-quality-factor light for being in porous structure
Microcavity is learned as detecting element, the transmission mechanism of excitation wavelength movement is caused using the deformation of gain media layer and variations in refractive index,
Compared to the detection method of quantum cascade laser, test macro is simple, at low cost, and Yi Shixian on piece is integrated, is miniaturized, just
The property taken is strong.
2, the present invention compares electricity gas sensing using the optical microcavity of Whispering-gallery-mode as basic sensing unit
Device, optical sensor it is low in energy consumption, electromagnetism interference is strong, and safety is good, strong flexibility.
3, the present invention can carry out molecular modification using gain medium materials, material molecule ends such as quantum dots to adsorb spy
Fixed gas molecule is advantageously implemented the specificity sensing of special gas, while convenient for expanding on piece low cost gas sensor
Type and function.
Detailed description of the invention
Fig. 1 is gas sensor of embodiment of the present invention fabrication processing schematic diagram.
Fig. 2 is a kind of gas sensor schematic diagram of the present invention.
Fig. 3 is gas sensor test system of embodiment of the present invention schematic diagram.
Fig. 4 is the gas sensor scanning electron microscope diagram piece of processing and fabricating of the present invention.
Fig. 5 is the gas sensor scanning electron microscope partial enlarged view of processing and fabricating of the present invention.
Fig. 6 is a kind of gas sensor preparation method flow chart of the present invention.
Wherein: 11-quartz glass plates；12-photoresists；13-polymeric layers；14-Colloidal Quantum Dots layers；21-pulses
Laser；22-plano-convex lens；23-gas chamber；24-gas outlets；25-air inlets one；26-air inlets two；27-filters
Mating plate；28-object lens；29-spectrometers；Device in 30-tests；31-light beams.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Whispering-gallery-mode is a kind of special electromagnetic wave mode of resonance being present in inside polygon resonator, is relied on humorous
Total internal reflection in device boundary face of shaking, can be passed with lesser optical loss along the arc microcavity surface of resonator
It broadcasts.Echo wall mode optical micro-cavity is made of high refractive index medium, and containment portion is then the medium of low-refraction, to utilize
High refractive index contrast is realized to the stronger constraint of electromagnetic wave.Its optical property primary article prime factor Q and mode volume V comes
Characterization, quality factor q reflect light wave and are bound in intracavitary energy size, it may also be said to be the service life of photon storage.Mode
Volume V reflects the effective volume for being strapped in intracavitary photon.Echo wall mode optical micro-cavity quality factor is high, mode volume is small
Feature makes it be widely used in the fields such as ray machine dynamics, quantum optices, biochemistry sensing, singular optics.In fact, logical
It crosses and selects suitable optical gain medium, specific micro-cavity structure is processed in design, it can be observed that different lasing phenomenons.It utilizes
The monitoring of different detection targets may be implemented in the transmission mechanism of lasing.Particularly, the physical chemistry of binding specificity gas sensing
Mechanism provides reliable guarantee, it can be achieved that high sensitivity, high-precision detection of gas for safety in production.
Embodiment one
As shown in Fig. 2, a kind of gas sensor based on polymer-doped type quantum dot gain medium, including it is patterned
There is ring-shaped groove on quartz glass substrate and polymer-doped quantum dot gain medium layer, quartz glass substrate surface.
The selection of polymer is on the one hand to improve the purity of quantum dot microcavity emission spectrum, on the other hand can be used as
Detect the absorbed layer of specific gas.After chamber pours under test gas, from transmission mechanism, Polymer absorption gas to be measured
It can be expanded after body, causing the microcavity of Whispering-gallery-mode, deformation occurs.Simultaneously as the absorption of gas molecule, causes micro-
The equivalent refractive index of cavity mold formula changes.The excitation wavelength of quantum dot microcavity can be all caused to send out in view of above two transmission mechanism
Raw movement, so saying that two kinds of mechanism enhance detection of gas when existing simultaneously from the angle that perception ambient atmos concentration changes
Sensitivity.
As shown in Figure 1, the above-mentioned gas sensor production method based on polymer-doped type quantum dot gain medium, specifically
Steps are as follows:
S1, the quartz glass plate 11 of 4 inch diameter sizes is selected to be used as substrate, and molten with the mixing of the concentrated sulfuric acid and hydrogen peroxide
Liquid is in 60 DEG C of cleaning 10min.
S2, spin coating negative photoresist KMPR12, thickness are about 14 μm, after 100 DEG C of front baking 6min, utilize Suss MA/BA-6
Type contact photoetching machine uv-exposure 60s；And then, 3min is dried after 100 DEG C, can obtain on a photoresist after being developed using TMAH
Obtain the mask pattern of micro-loop shape.
S3, using reactive ion glass etching equipment, using photoetching offset plate figure as exposure mask, by C4F8With both etchings of He
Gas carries out dry etching to quartz glass, it is desirable that sidewall profile is smooth steep；Wherein, chamber pressure is set as 4mTorr, line
Circle power is 1400W, platen power 300W, C4F8Flow velocity with He is respectively 10sccm and 174sccm, finally utilizes acetone
The transfer processing of quartz glass substrate on piece micro-loop figure can be completed after ultrasonic depolymerization.
S4, the small pieces that quartz glass substrate is cut into 1cm × 1cm size are prepared into deposition increasing with commercial scribing machine ADT7100
Beneficial dielectric material.
S5, by polystyrene PS grain dissolution in toluene solvant, be configured to mass fraction be 3% clear solution A；It will
CdSe/ZnS core-shell quanta dots are dispersed in toluene solvant, be configured to concentration be 30mg/mL dispersion liquid B, later by solution A with
B solution is mixed and made into polymer-doped quantum dot gain medium material according to volume ratio 1:9.
S6, the resulting quantum dot gain medium of spin-coating step S5, revolving speed 900rpm, time 40s, 130 DEG C of front baking 15min
The quantum dot gain medium film of curable polymer doping afterwards is completed one and is situated between based on polymer P S doping type quantum dot gain
The gas sensor blank of matter makes, which can be used for detecting ethyl alcohol, methanol, acetone, the gas concentrations such as isopropanol.
Fig. 3 show the corresponding test macro schematic diagram of the present invention.The test macro specifically includes that 21-pulse lasers
Device；22-plano-convex lens；23-gas chamber；27-optical filters；28-object lens；29-spectrometers；Device in 30-tests,
31-light beams.Wherein, gas chamber includes three ports, two air inlets 25,26, a gas outlet 24.When device detection, arteries and veins
The free space optical for rushing laser sending first passes around lens focus to microcavity sample surfaces, spot diameter about 300um, gain
The optical signal that dielectric layer scatters out is collected after object lens focus by spectrometer.When gas concentration changes, gain is situated between
The corresponding excitation wavelength of matter layer can move, and by the spectrogram on comparison spectrometer, the survey of gas concentration variation can be completed
Amount.
In this implementation case, KMPR photoresist is a photoresist of MicroChem company, the U.S., is belonged to common on the market
A kind of product, etch resistance is strong, and steepness is good.
Embodiment two
As shown in Fig. 2, a kind of gas sensor based on polymer-doped type quantum dot gain medium, including it is patterned
There is ring-shaped groove on quartz glass substrate and polymer-doped quantum dot gain medium layer, quartz glass substrate surface.
As shown in Figure 1, the above-mentioned gas sensor production method based on polymer-doped type quantum dot gain medium, specifically
Steps are as follows:
S1, select the quartz glass plate of 4 inch diameter sizes as substrate, and with the mixed solution of the concentrated sulfuric acid and hydrogen peroxide
In 60 DEG C of cleaning 10min.
S2, spin coating negative photoresist KMPR, thickness are about 14 μm, after 100 DEG C of front baking 6min, utilize Suss MA/BA-6 type
Contact photoetching machine uv-exposure 60s；And then, 3min is dried after 100 DEG C, can obtain on a photoresist after being developed using TMAH
The mask pattern of micro-loop shape.
S3, using reactive ion glass etching equipment, using photoetching offset plate figure as exposure mask, by C4F8With both etchings of He
Gas carries out dry etching to quartz glass, it is desirable that sidewall profile is smooth steep；Wherein, chamber pressure is set as 4mTorr, line
Circle power is 1400W, platen power 300W, C4F8Flow velocity with He is respectively 10sccm and 174sccm, finally utilizes acetone
The transfer processing of quartz glass substrate on piece micro-loop figure can be completed after ultrasonic depolymerization.
S4, the small pieces that quartz glass substrate is cut into 1cm × 1cm size are prepared into deposition increasing with commercial scribing machine ADT7100
Beneficial dielectric material.
S5, by polymetylmethacrylate grain dissolution in toluene solvant, be configured to mass fraction be 3% it is saturating
Bright solution A；CdSe/ZnS core-shell quanta dots are dispersed in toluene solvant, the dispersion liquid B that concentration is 30mg/mL is configured to, it
Solution A and B solution are mixed and made into polymer-doped quantum dot gain medium material according to volume ratio 2:8 afterwards.
S6, the resulting quantum dot gain medium of spin-coating step S5, revolving speed 900rpm, time 40s, 130 DEG C of front baking 15min
The quantum dot gain medium film of curable polymer doping afterwards completes one based on polymer P MMA doping type quantum dot microcavity
The production of gas sensor blank, which can be used for detecting vapor, the gas concentrations such as ammonia.
The corresponding test macro of the present embodiment and testing procedure are the same as example 1.
Embodiment three
As shown in Fig. 2, a kind of gas sensor based on polymer-doped type quantum dot gain medium, including it is patterned
There is ring-shaped groove on quartz glass substrate and polymer-doped quantum dot gain medium layer, quartz glass substrate surface.
As shown in Figure 1, the above-mentioned gas sensor production method based on polymer-doped type quantum dot microcavity, specific steps
It is as follows:
S1, select the quartz glass plate of 4 inch diameter sizes as substrate, and with the mixed solution of the concentrated sulfuric acid and hydrogen peroxide
In 60 DEG C of cleaning 10min.
S2, spin coating negative photoresist KMPR, thickness are about 14 μm, after 100 DEG C of front baking 6min, utilize Suss MA/BA-6 type
Contact photoetching machine uv-exposure 60s；And then, 3min is dried after 100 DEG C, can obtain on a photoresist after being developed using TMAH
The mask pattern of micro-loop shape.
S3, using reactive ion glass etching equipment, using photoetching offset plate figure as exposure mask, by C4F8With both etchings of He
Gas carries out dry etching to quartz glass, it is desirable that sidewall profile is smooth steep；Wherein, chamber pressure is set as 4mTorr, line
Circle power is 1400W, platen power 300W, C4F8Flow velocity with He is respectively 10sccm and 174sccm, finally utilizes acetone
The transfer processing of quartz glass substrate on piece micro-loop figure can be completed after ultrasonic depolymerization.
S4, the small pieces that quartz glass substrate is cut into 1cm × 1cm size are prepared into deposition increasing with commercial scribing machine ADT7100
Beneficial dielectric material.
S5, by polyethyleneimine PEI grain dissolution in toluene solvant, be configured to mass fraction be 3% clear solution
A；CdSe/ZnS core-shell quanta dots are dispersed in toluene solvant, the dispersion liquid B that concentration is 30mg/mL is configured to, it is later that A is molten
Liquid and B solution are mixed and made into polymer-doped quantum dot gain medium material according to volume ratio 1.5:8.5.
S6, the resulting quantum dot gain medium of spin-coating step S5, revolving speed 900rpm, time 40s, 130 DEG C of front baking 15min
The quantum dot gain medium film of curable polymer doping afterwards completes one based on polymer P EI doping type quantum dot microcavity
The production of gas sensor blank, which can be used for detecting the gas concentrations such as carbon dioxide, vapor.
The corresponding test macro of the present embodiment and testing procedure are the same as example 1.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of gas sensor, which is characterized in that including substrate and the gain media layer being deposited on substrate；Substrate surface has
Ring-shaped groove.
2. gas sensor according to claim 1, which is characterized in that the substrate is quartz glass substrate, with a thickness of
5um-4mm, it is 0.1um-500um, etching depth 0.1um-500um that ring-shaped groove, which etches width,.
3. gas sensor according to claim 3, which is characterized in that the gain media layer includes Colloidal Quantum Dots layer
Cured polymeric layer thereon, the thickness of gain media layer is between 0.1um-500um.
4. gas sensor according to claim 3, which is characterized in that the quantum dot of the Colloidal Quantum Dots layer is binary
Or the monokaryon quantum dot of ternary or quaternary, or be the core-shell type quantum point of binary or ternary or quaternary, or for surface hydroxylation or
Quantum dot gain material after amination functionalized modification；The concentration of quantum dot is 1mg/mL-100mg/mL；The polymeric layer
Polymer is thermoplastics type's light functional polymer material；Polymer-doped mass fraction is 0.1%-10%.
5. a kind of gas sensor preparation method, which is characterized in that specifically include following step:
S1, ring-shaped groove is processed as gas sensor main body on quartz glass substrate surface using lithographic etch process；
S2, the quantum dot that deposited polymer adulterates in gas sensor main body are completed to be based on piece amount as gain media layer
The gas sensor production of son point microcavity.
6. preparation method according to claim 5, which is characterized in that the step S1 choosing is with a thickness of 5um-4mm, surface light
Sliding smooth quartz glass substrate processes ring-shaped groove on quartz glass substrate surface using the method for semiconductor lithography etching.
7. preparation method according to claim 6, which is characterized in that for quartz glass substrate on piece ring in the step S1
The chemical wet etching of shape groove, the etching width of ring-shaped groove are 0.1um-500um, etching depth 0.1um-500um；Etched line
It encloses power and is lower than 2000W, radio-frequency power is lower than 1000W, etching gas C4F8Flow velocity is lower than 100sccm, and He flow velocity is lower than
30sccm。
8. preparation method according to claim 5, which is characterized in that the step S2 is deposited in gas sensor main body
The processing step of polymer-doped quantum dot gain medium are as follows: it is molten with Colloidal Quantum Dots to mix a certain amount of polymer first
Liquid, it is desirable that mixed solution is evenly distributed, and does not precipitate, and deposits gain medium material using the method for spin coating later, after solidification i.e.
The achievable gas sensor prototype based on quantum dot microcavity.
9. preparation method according to claim 8, which is characterized in that the step S2 is selected as thermoplastics type to polymer
Light functional polymer material；Polymer-doped mass fraction is 0.1%-10%；
Colloidal Quantum Dots layer choosing selects the monokaryon quantum dot of binary or ternary or quaternary, or the nucleocapsid of selection binary or ternary or quaternary
Quantum dot gain material after type quantum dot, or selection surface hydroxylation or amination functionalized modification；The concentration of quantum dot controls
In 1mg/mL-100mg/mL；The thickness of the quantum dot gain medium of the deposited polymer doping is between 0.1um-500um.
10. preparation method according to claim 5, which is characterized in that the gain media selects organic dyestuff or organic
Dye composition or rare earth ion or rare earth ion compound or semiconducting organic polymer or pure quantum dot or quantum dot are compound
Object.
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| CN110231485A (en) * | 2019-07-08 | 2019-09-13 | 北方民族大学 | A kind of biosensor and preparation method thereof |
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