CN107389616B - A kind of sensor chip and preparation method thereof - Google Patents
A kind of sensor chip and preparation method thereof Download PDFInfo
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- CN107389616B CN107389616B CN201710428834.6A CN201710428834A CN107389616B CN 107389616 B CN107389616 B CN 107389616B CN 201710428834 A CN201710428834 A CN 201710428834A CN 107389616 B CN107389616 B CN 107389616B
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Abstract
The present invention relates to a kind of sensor chips and preparation method thereof, belong to surface plasma resonance sensor chip design preparation technical field.The chip is composite construction made of being arranged successively from the bottom to top as the laminated film of glass substrate, metal film, self-assembled film and metal oxide and polymer, nano-metal-oxide is successfully fixed on by sensor chip surface using the method that polymer embeds, effectively raises detection range and sensitivity to object gas.Method of the present invention is simple, and prepared sensor chip has good sensitivity to sulfur dioxide and meets the requirement detected under normal temperature conditions, has good response signal in 5ppm~40ppm.
Description
Technical field
The present invention relates to a kind of sensor chips and preparation method thereof, belong to surface plasma body resonant vibration (Surface
Plasmon resonance, SPR) sensor chip design preparation technical field.
Background technique
In an atmosphere, sulfur dioxide can aoxidize to form sulfate aerosol, be the important predecessor of environmental acidification.Work as atmosphere
When middle sulfur dioxide concentration is reached for 0.21ppm, respiratory disease disease incidence can be made to increase, therefore needed in real-time monitoring environment
Sulfur dioxide concentration tool.Currently, being more common in electrochemical sensor and optics for the sensor of sulfur dioxide gas
Sensor is then seldom.
As an important representative of optical sensor, surface plasmon resonance sensor is capable of providing online real-time
Monitoring data provides effective tool for pernicious gas in real-time monitoring environment.Surface plasmon wave resonance is a kind of light
Phenomenon is learned, it is extremely sensitive to the variation of the dielectric constant of metal surface, dielectric thickness, refractive index.In general physics or
The dielectric dielectric constant, thickness, refractive index that chemical change can influence metal surface change.Surface plasma
Wave resonance sensor has the characteristics that real-time, dynamic, high sensitivity, sample without marking.Therefore, total based on surface plasma
The sensor of vibration technology has been widely used in the every field such as drug development, food safety, environmental monitoring.But surface
Application of the plasma wave resonance sensor in gas detection also faces problems, and core is exactly preparation for certain
The sensor chip of gas.Uniform nano-scale sensitive membrane how is be effectivelyed prepared on surface plasma chip, is formed
Sensor chip makes sensor keep having quick, highly sensitive, stable response signal to sulfur dioxide under normal temperature conditions
Characteristic needs suitable film-forming method, and to filming technology, higher requirements are also raised.
At present for the material of the seldom reason of the optics sensor of sulfur dioxide and absorption sulfur dioxide gas molecule
Not onrelevant.The reported material about absorption sulfur dioxide gas molecule mainly has metal oxide, ionic liquid, polymerization
Object, organic metal framework.In recent years, the metal oxides such as tin oxide, iron oxide, titanium dioxide are used for gas as adsorbent material
Detection has obtained extensive concern, especially titanium dioxide, this is because titanium dioxide has the surface chemical property of soda acid both sexes,
The acid/base on its easily controllable surface is reacted.The metal-oxide film surface of conventional method preparation has with what gas molecule acted on
Imitate limited area, it is therefore desirable to improve its adsorption efficiency by improving the contact area of metal oxide and gas molecule.It receives
Rice corpuscles specific surface area with higher, can be used for solving the above problems, but how that nanoparticle abundant is effectively solid
Surely arriving sensor surface is still a hot issue.
Summary of the invention
It detects existing for sulfur dioxide and asks under normal temperature conditions for existing surface plasma resonance sensor chip
Topic, the purpose of the present invention is to provide a kind of sensor chip and preparation method thereof, the chip has sulfur dioxide fine
Sensitivity and meet the requirement that is detected under normal temperature conditions, there is good response signal in 5ppm~40ppm；It is first
It is first self-assembled modified to the metal film progress of glass substrate surface deposition, then prepared on self-assembled film by way of thermal polymerization
Polymer composite film containing metal nanoparticle, to obtain the chip.
Mesh of the invention is achieved through the following technical solutions:
A kind of sensor chip, the chip are by glass substrate, metal film, self-assembled film and metal oxide and to gather
Composite construction made of the laminated film of conjunction object is arranged successively from the bottom to top.
The metal film includes aluminium film, silverskin or golden film, preferably golden film；Preferred 40nm~the 50nm of the thickness of metal film.
The self assembly liquid for preparing the self-assembled film is sulfydryl acrylic acid, mercaptoethylmaine or mercaptan, and the chemical formula of mercaptan is
HS(CH2)nCH3, n=5~18；
In the laminated film of the metal oxide and polymer, metal oxide is that grain diameter is 5nm~10nm
Titanium dioxide, di-iron trioxide, aluminium oxide, nickel oxide or tin oxide, polymer are polymethylacrylic acid, polyacrylic acid, poly- first
One of base hydroxy-ethyl acrylate, polyacrylamide.
A kind of preparation method of sensor chip of the present invention, the method comprises the following steps:
Step 1. plates layer of metal film using the method for vacuum evaporation on a glass substrate；
Glass substrate after deposited metal film is placed in the self assembly liquid that concentration is 0.1mmol/L~1mmol/L by step 2.
Glass substrate rinsing, drying after taking out in self assembly liquid is formed self-assembled film by middle immersion 12h~72h on metal film；
Step 3. is by metal oxide dispersion to purity not less than in the water of deionized water, and ultrasound mixes, and obtaining concentration is
10-7Mol/L~10-5The aaerosol solution of mol/L；
Step 4. is by function monomer, crosslinking agent and initiator by 1:(0.1~6): the mass ratio of (0.1~1) mixes
It closes, and ultrasonic degassing, obtains mixed solution I；
Step 5. is mixed aaerosol solution with mixed solution I by the volume ratio of 1~3:20, first carries out ultrasonic degassing,
Lead to nitrogen 3min or more again, obtains mixed solution II；
Step 6. forms one along one circle parafilm of the periphery of self-assembled film paste between parafilm and self-assembled film
Groove；Then, mixed solution II is added in groove, then places the sheet glass of silanization on parafilm, make para
A closed reaction compartment is formed between the sheet glass of film, self-assembled film and silanization；It again will be empty with closed reaction
Between glass substrate be placed in the reaction vessel for being filled with protective gas, at 50 DEG C~80 DEG C react 3h~12h, in self-assembled film
The upper laminated film for forming metal oxide and polymer；Finally, removing the sheet glass and parafilm of silanization, contain gold
The glass substrate of the laminated film of category oxide and polymer, self-assembled film and metal film is the chip；
The function monomer is methacrylic acid, acrylic acid, hydroxyethyl methacrylate or acrylamide, and function monomer
Concentration in mixed solution I is 10mmol/L~550mmol/L；
The crosslinking agent is N, N '-methylene-bisacrylamide, ethylene glycol dimethacrylate, trimethylolpropane tris
Methacrylate, pentaerythritol triacrylate or pentaerythritol tetraacrylate；
The initiator is azodiisobutyronitrile or potassium peroxydisulfate；
The protective gas includes nitrogen or argon gas.
In step 2, the preferred 1mmol/L of the concentration of self assembly liquid, soaking time is preferably for 24 hours.
In step 3, the amount of the mixed solution II in reaction tank is added to fill up closed reaction compartment.
The utility model has the advantages that
Nano-metal-oxide is successfully fixed on sensor chip surface using the method for polymer embedding by the present invention,
The detection range and sensitivity to object gas are effectively raised, this is because metal oxide nanoparticles surface is special
Chemical property and higher specific surface area can be acted on effectively with object gas, while using thin polymer film as support
Suitable metal oxide nanoparticles are embedded by object, under the premise of keeping its permeability, and enrich nanoparticle
Quantity increases action site；Moreover, prepared sensor chip has good sensitivity to sulfur dioxide and meets
The requirement detected under normal temperature condition has good response signal, and side of the present invention in 5ppm~40ppm
Method is simple.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of sensor chip of the present invention.
Fig. 2 is the structural schematic diagram of closed reaction compartment of the present invention.
Fig. 3 is the SPR curve graph adsorbed before and after 5ppm sulfur dioxide using sensor chip prepared in embodiment 1.
Fig. 4 is the SPR curve graph adsorbed before and after 5ppm sulfur dioxide using sensor chip prepared in embodiment 2.
Wherein, 1- glass substrate, 2- metal film, 3- self-assembled film, the laminated film of 4- metal oxide and polymer, 5-
Parafilm, the sheet glass of 6- silanization.
Specific embodiment
The present invention will be further described With reference to embodiment.
In following embodiment:
Glass substrate: the LaSFN9 glass that refractive index is 1.845；
It is 0.9999 that golden purity used in golden film, which is deposited,；
Allyl sulfhydrate: 70wt%, lark prestige Science and Technology Ltd.；
Mercaptoethylmaine: 95wt%, Shanghai Aladdin biochemical technology limited liability company；
Titanium dioxide: anatase titanium dioxide, grain diameter 5nm~10nm, Shanghai Aladdin biochemical technology share are limited
Company；
The purity of high pure nitrogen is greater than 99.99%；
The sheet glass of the silanization is the sheet glass of trim,ethylchlorosilane silanization；
The metal film is golden film.
Embodiment 1
As shown in Figure 1, a kind of sensor chip is from the bottom to top successively by glass substrate 1, metal film 2, self-assembled film 3 and gold
The laminated film 4 for belonging to oxide and polymer forms, and specific preparation process is as follows for the sensor chip:
Step 1. uses the method for vacuum evaporation to plate a layer thickness in glass substrate 1 as the metal film 2 of 49nm；
Glass substrate 1 after deposited metal film 2 is placed in the allyl sulfhydrate that concentration is 1mmol/L by step 2., static
After placing for 24 hours, glass substrate 1 is taken out from allyl sulfhydrate, rinsed with dehydrated alcohol and dried up with high pure nitrogen, in metal
Self-assembled film 3 is formed on film 2；
Titanium dioxide powder is distributed in distilled water step 3. and ultrasound mixes, and obtaining concentration is 1 × 10-6Mol/L's
Aaerosol solution；
Step 4. is by 0.0355g acrylamide, 0.0062g N, N '-methylene-bisacrylamide and contains 0.0041g
950 μ L aqueous solutions of potassium peroxydisulfate are mixed, and ultrasonic degassing 10min, obtain mixed solution I；
50 μ L aaerosol solutions are added in 950 μ L mixed solutions I by step 5., first carry out ultrasonic degassing 10min, then logical nitrogen
Gas 5min obtains mixed solution II；
Step 6. is formed between parafilm 5 and self-assembled film 3 along one circle parafilm 5 of the periphery of self-assembled film 3 paste
One groove；Then, mixed solution II is added in groove, then places the sheet glass 6 of silanization on parafilm 5, made
A closed reaction compartment is formed between the sheet glass 6 of parafilm 5, self-assembled film 3 and silanization, is detailed in Fig. 2；Again will
Glass substrate 1 with closed reaction compartment is placed in the sealing flat bottom glass reaction vessel for being filled with high pure nitrogen, at 75 DEG C
Lower reaction 8h forms the laminated film 4 of metal oxide and polymer on self-assembled film 3；Finally, removing the glass of silanization
Piece 6 and parafilm 5, the glass of laminated film 4, self-assembled film 3 and metal film 2 containing metal oxide and polymer
Substrate 1 is the sensor chip.
Sensor chip prepared by the present embodiment is installed into the reaction tank of surface plasmon wave resonance detection device,
Surface plasmon wave resonance structure is constituted, by measuring the reflective light intensity after being incident on sensor chip surface reflection with incidence
The curve of angular variation, i.e. SPR curve, the SPR curve before being adsorbed；It is subsequently passed the sulfur dioxide of 5ppm, is surveyed again
SPR curve after measuring absorption, as shown in Figure 3.Resonance angle angle (the i.e. corresponding angle of incident light of light intensity minimum value before adsorbing
Degree) it is 49.98 °, resonance angle angle increases to 50.16 ° after adsorbing 3.5min, and the increase of resonance angle shows with sulfur dioxide
Be passed through, constantly there is gas molecule to enter in the metal oxide of sensor chip surface and the laminated film 4 of polymer, and with
The titanium dioxide nano-particle effect for being included, makes the dielectric constant on surface change, and resonance angle is caused to increase.
Embodiment 2
A kind of sensor chip from the bottom to top successively by glass substrate 1, metal film 2, self-assembled film 3 and metal oxide with
The laminated film 4 of polymer forms, and specific preparation process is as follows for the sensor chip:
Step 1. uses the method for vacuum evaporation to plate a layer thickness in glass substrate 1 as the metal film 2 of 45nm；
Glass substrate 1 after deposited metal film 2 is placed in the mercaptoethylmaine that concentration is 0.1mmol/L by step 2., static
After placing 12h, glass substrate 1 is taken out from mercaptoethylmaine, rinsed with dehydrated alcohol and dried up with high pure nitrogen, in metal film
Self-assembled film 3 is formed on 2；
Titanium dioxide powder is distributed in distilled water step 3. and ultrasound mixes, and obtaining concentration is 1 × 10-7Mol/L's
Aaerosol solution；
Step 4. is by 0.0086g methacrylic acid, 0.0344g ethylene glycol dimethacrylate and contains 0.002g idol
900 μ L acetonitrile solutions of nitrogen bis-isobutyronitrile are mixed, and ultrasonic degassing 10min, obtain mixed solution I；
100 μ L aaerosol solutions are added in 900 μ L mixed solutions I by step 5., first carry out ultrasonic degassing 10min, then lead to
Nitrogen 5min obtains mixed solution II；
Step 6. is formed between parafilm 5 and self-assembled film 3 along one circle parafilm 5 of the periphery of self-assembled film 3 paste
One groove；Then, mixed solution II is added in groove, then places the sheet glass 6 of silanization on parafilm 5, made
A closed reaction compartment is formed between the sheet glass 6 of parafilm 5, self-assembled film 3 and silanization；To have again closed
The glass substrate 1 of reaction compartment be placed in the sealing flat bottom glass reaction vessel for being filled with high pure nitrogen, reacted at 70 DEG C
12h forms the laminated film 4 of metal oxide and polymer on self-assembled film 3；Finally, remove the sheet glass 6 of silanization with
And parafilm 5, the glass substrate 1 of laminated film 4, self-assembled film 3 and metal film 2 containing metal oxide and polymer
The as described sensor chip.
Sensor chip prepared by the present embodiment is installed into the reaction tank of surface plasmon wave resonance detection device,
Surface plasmon wave resonance structure is constituted, and measures the SPR curve before and after absorption sulfur dioxide.As can be seen from FIG. 4, before absorption
Resonance angle angle (i.e. the corresponding incident light angle of light intensity minimum value) is 48.85 °, and resonance angle angle increases to after adsorbing 4min
49.03 °, the increase of resonance angle shows being passed through with sulfur dioxide, constantly has gas molecule to enter sensor chip surface
Metal oxide and polymer laminated film 4 in, and with included titanium dioxide nano-particle act on, make Jie on surface
Electric constant changes, and resonance angle is caused to increase.
In conclusion the above is merely preferred embodiments of the present invention, being not intended to limit the scope of the present invention.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (5)
1. a kind of sensor chip, it is characterised in that: the chip is by glass substrate (1), metal film (2), self-assembled film (3)
And the laminated film (4) of metal oxide and polymer be arranged successively from the bottom to top made of composite construction；
The metal film (2) includes aluminium film, silverskin or golden film；
The self assembly liquid for preparing the self-assembled film (3) is sulfydryl acrylic acid, mercaptoethylmaine or mercaptan；Wherein, the chemistry of mercaptan
Formula is HS (CH2)nCH3, n=5~18；
In the laminated film (4) of the metal oxide and polymer, metal oxide is two that grain diameter is 5nm~10nm
Titanium oxide, di-iron trioxide, aluminium oxide, nickel oxide or tin oxide；Polymer is polymethylacrylic acid, polyacrylic acid, poly- methyl
Hydroxy-ethyl acrylate or polyacrylamide.
2. a kind of sensor chip according to claim 1, it is characterised in that: the metal film (2) with a thickness of 40nm
~50nm.
3. a kind of preparation method of sensor chip as claimed in claim 1 or 2, it is characterised in that: the method step is such as
Under:
Step 1. plates layer of metal film (2) using the method for vacuum evaporation on glass substrate (1)；
Glass substrate (1) after deposited metal film (2) is placed in the self assembly that concentration is 0.1mmol/L~1mmol/L by step 2.
12h~72h is impregnated in liquid, and glass substrate (1) rinsing, drying after taking out in self assembly liquid is formed certainly on metal film (2)
Assembling film (3)；
By metal oxide dispersion to purity not less than in the water of deionized water, ultrasound mixes step 3., and obtaining concentration is 10- 7Mol/L~10-5The aaerosol solution of mol/L；
Step 4. is by function monomer, crosslinking agent and initiator by 1:(0.1~6): the mass ratio of (0.1~1) mixes, and
Ultrasonic degassing obtains mixed solution I；
Step 5. is mixed aaerosol solution with mixed solution I by the volume ratio of 1~3:20, first carries out ultrasonic degassing, then lead to
Nitrogen 3min or more obtains mixed solution II；
Step 6. is along one circle parafilm (5) of the periphery of self-assembled film (3) paste, between parafilm (5) and self-assembled film (3)
Form a groove；Then, mixed solution II is added in groove, then places the glass of silanization on parafilm (5)
Piece (6) makes to form a closed reaction sky between the sheet glass (6) of parafilm (5), self-assembled film (3) and silanization
Between；The glass substrate (1) with closed reaction compartment is placed in the reaction vessel for being filled with protective gas again, 50 DEG C~80
3h~12h is reacted at DEG C, and the laminated film (4) of metal oxide and polymer is formed on self-assembled film (3)；Finally, removing
The sheet glass (6) and parafilm (5) of silanization, laminated film (4), self-assembled film containing metal oxide and polymer
(3) and the glass substrate (1) of metal film (2) is the chip；
The function monomer is methacrylic acid, acrylic acid, hydroxyethyl methacrylate or acrylamide；
The crosslinking agent is N, N '-methylene-bisacrylamide, ethylene glycol dimethacrylate, trimethylol propane trimethyl
Acrylate, pentaerythritol triacrylate or pentaerythritol tetraacrylate；
The initiator is azodiisobutyronitrile or potassium peroxydisulfate；
The protective gas includes nitrogen or argon gas.
4. a kind of preparation method of sensor chip according to claim 3, it is characterised in that: in step 2, self assembly liquid
Concentration be 1mmol/L, soaking time be for 24 hours.
5. a kind of preparation method of sensor chip according to claim 3, it is characterised in that: in step 4, function monomer
Concentration in mixed solution I is 10mmol/L~550mmol/L.
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| CN108169428B (en) * | 2017-12-29 | 2020-11-27 | 华南师范大学 | Formaldehyde gas, humidity and temperature integrated monitoring equipment |
| CN112711090B (en) * | 2020-12-17 | 2022-07-15 | 山东省科学院生物研究所 | Method for regulating LPFG sensitivity by polymethacrylic acid |
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| EP2071321A3 (en) * | 2007-12-13 | 2009-09-09 | Fujifilm Corporation | Surface plasmon resonance biosensor |
| CN104897617A (en) * | 2015-05-19 | 2015-09-09 | 国家纳米科学中心 | Micro-array biochip, and preparation method and application of micro-array biochip |
| CN106124457A (en) * | 2016-06-17 | 2016-11-16 | 北京理工大学 | A kind of preparation method of surface plasma resonance sensor chip based on nano material |
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| US20070222995A1 (en) * | 2006-03-27 | 2007-09-27 | Jennifer Lu | Artifact having a textured metal surface with nanometer-scale features and method for fabricating same |
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|---|---|---|---|---|
| EP2071321A3 (en) * | 2007-12-13 | 2009-09-09 | Fujifilm Corporation | Surface plasmon resonance biosensor |
| CN104897617A (en) * | 2015-05-19 | 2015-09-09 | 国家纳米科学中心 | Micro-array biochip, and preparation method and application of micro-array biochip |
| CN106124457A (en) * | 2016-06-17 | 2016-11-16 | 北京理工大学 | A kind of preparation method of surface plasma resonance sensor chip based on nano material |
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