CN109900667A - A kind of selectively super quick biochemical sensor of full optical fiber laser type - Google Patents
A kind of selectively super quick biochemical sensor of full optical fiber laser type Download PDFInfo
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- CN109900667A CN109900667A CN201910198450.9A CN201910198450A CN109900667A CN 109900667 A CN109900667 A CN 109900667A CN 201910198450 A CN201910198450 A CN 201910198450A CN 109900667 A CN109900667 A CN 109900667A
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Abstract
The present invention relates to optical sensing, material science and biochemical sensitive fields, are related to optical sensing and microcavity sensing technology, specifically provide a kind of selectively super quick biochemical sensor of full optical fiber laser type；Present invention integrated functionality graphene oxide film in quartz capillary, dielectric material as sensing, by the fluorescence resonance transfer characteristic of functional graphene oxide and advanced heterodyne detection and phase lock amplifying technology, while realizing functionalized sensing external world biochemical molecular, the sensing sensitivity of biochemical sensor is greatly improved, sensing sensitivity can reach unimolecule magnitude；Meanwhile the biochemical sensor is highly reliable, resists that anti-interference, signal-to-noise ratio is high, which can be directly integrated in all optical fiber system, realize the array detection of biochemical sensitive.
Description
Technical field
The present invention relates to optical sensing, material science and biochemical sensitive fields, are related to optical sensing and microcavity sensing technology,
A kind of selectively super quick biochemical sensor of full optical fiber laser type is specifically provided.
Background technique
With the development that optical sensing technology is maked rapid progress, optical sensor obtains rapid progress.Light wave passes in the waveguide
Sowing time, characterize the characteristic parameter (amplitude, phase, polarization state, wavelength etc.) of light wave because extraneous factor (such as temperature, pressure, magnetic field,
Electric field, displacement, rotation etc.) effect and change, so as to detect various physical quantitys on the optical sensor.With tradition
Sensor compare, there is optical sensor transmitting to contain much information, anti-electromagnetic interference capability is strong, safe and reliable, high sensitivity, can
The advantages that constituting sensing network, and the place that human hazard or the mankind can not be reached in high-temperature region, nuclear radiation area etc.
Work；Therefore, optical sensor is increasingly valued by people, and is widely used in building structure, instrument and meter, biology doctor
The fields such as treatment, oil exploration.Currently, main optical sensor product is limited with probing wave length in the market, responsiveness is not high,
Structure is complicated Deng flaws, be applied to bio-sensing field when, to sensor-based system propose small size, strong antijamming capability, can
Good, high sensitivity the rigors by property.
Although optical micro-cavity sensors size is smaller, micron dimension can reach, and there is high quality factor, then
Possess high sensitivity；But optical micro-cavity sensors are applied to biochemical sensitive field and need to overcome many obstacles: laser coupled
Stability and follow up device integration packaging, and the selectivity of biochemical molecular to be measured is distinguished；Therefore, to a certain extent
Limit its application face and practicability.
It is fluorescence detection that another biochemical sensitive field, which commonly senses means,；Fluorescence analysis method due to high sensitivity,
Selectivity is good, needs the features such as few sample amount, fast and easy, using very extensive in biochemical sensitive and analysis detection, as environment is supervised
Survey, food safety inspection and diagnostic analysis of the relevant physical signs of human body diseases etc..But fluorescence detection there are it is several not
Evitable problem, for example, it is desired to which related substances are marked, label is with high costs, while mark molecule will certainly be to life
The reaction process of chemoattractant molecule generates certain influence；In addition, not high in fluorescence detection medium sensitivity, detection accuracy is commonly micro-
Meter level is other, is unable to reach unimolecule magnitude, therefore limits its further application.
Graphene oxide is a kind of important derivatives of graphene, is the presoma that chemical reduction method prepares graphene, together
There are a variety of oxygen-containing functional groups, such as carboxyl, hydroxyl, epoxy group etc. at the edge and surface of Shi Qi lamellar structure；Also exactly by
In the presence of the oxygen-containing functional group make functional graphene oxide than graphene it is water-soluble more preferably；In addition functionalization aoxidizes stone
Black alkene has the conjugated structure of large area, can be used as energy acceptor and quenches to a variety of organic dyestuff, compared to traditional
Quencher, graphene oxide have higher quenching efficiency.
Based on this, the selectively super quick life of the full optical fiber laser type based on functional graphene oxide that the invention proposes a kind of
Change sensor.By functional graphene oxide thin-film integration in microcavity sensors inside cavity, get rid of traditional based on fluorescence
The limitation without chamber sensing of biochemistry detection, compared with traditional microcavity sensors, the present invention is in addition to the spy with microcavity sensors
It surveys outside the high advantage of sensitivity, also its function of sensing parameter selection is expanded, can be had for different molecular
Super quick selectivity analysis solves the problems, such as that selectivity senses biochemical molecular to be measured and cannot take into account with unimolecule hypersensitivity.
Summary of the invention
It is an object of the invention in view of the above problems or insufficient, to solve existing biochemical sensor fluorescence mark
Remember that at high price, sensing accuracy is not high, the selectivity of functionalization realizes the problems such as difficulty is big, the present invention provides one kind to be based on function
The selectively super quick biochemical sensor of full optical fiber laser type that graphene oxide can be changed is improved intracavitary using Fa-Po cavity body structure
The effect number of photon and intracavitary biochemical molecular to be measured will be intracavitary using the graphene oxide film of functionalization as sensitive layer
It is passed through the mixed liquor of biochemical molecular solution and rhodamine solution to be measured, using different biochemical moleculars and is adhered to functionalization oxygen
The competitive effect of the rhodamine molecule of graphite alkene film, so that rhodamine molecule takes off on functional graphene oxide film
It falls, generates fluorescence reproduction in a free state, hereafter photon continuous gain amplification in method amber resonant cavity generates laser signal, light
After electricity conversion, electricity sensing testing system is accessed, the extraction and measurement of signal are completed using heterodyne detection and phase lock amplifying technology.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of selectively super quick biochemical sensor of full optical fiber laser type, comprising: 1 quartz capillary and 2 single mode optical fibers；
It is characterized in that, the inner wall of the quartz capillary is attached with functional graphene oxide film；The every single mode optical fiber
Golden film is deposited on the end face of one end, 2 single mode optical fibers are plugged in the quartz capillary, altogether with mode of the golden film end face in
With composition Fa-Po cavity structure；The functional graphene oxide film is by partial reduction graphene oxide film surface adhesion H+、
OH-Or Na+It is formed after ion.
Further, the cavity of the Fa-Po cavity structure is used to store the mixed of biochemical molecular solution to be measured and rhodamine liquor
Close liquid, the golden film end face mechanics amber microcavity of mixed liquor and both ends single mode optical fiber, Q value >=500,000 of the method amber microcavity.
Further, the cavity length of the Fa-Po cavity structure is 5~8 millimeters；The golden film end face of i.e. 2 single mode optical fibers it
Between spacing be 5~8 millimeters.
Further, thickness >=30 nanometer of the golden film, in reflectivity >=80% of visible light wave range.
Further, the preparation method of the functional graphene oxide film, comprising the following steps:
Quartz capillary is dipped vertically into the graphene oxide dispersion of 0.5~3g/L by step 1, is made using capillary
With absorption graphene oxide dispersion；
Step 2 will inhale the quartz capillary drying for having graphene oxide dispersion, soak quartz capillary after the completion of drying
Enter to keep temperature water bath's heating 20 minutes or more of 60~80 DEG C in the VC solution of 20~50g/L, reduction process to aoxidize stone
Black alkene becomes partial reduction graphene oxide after VC is restored；
Step 3 is cleaned in quartz capillary with clear water and again dries quartz capillary after remaining VC solution, obtains interior
Wall is attached with the quartz capillary of partial reduction graphene oxide film；
Step 4, nitric acid solution, the ammonium hydroxide of PH=8 or the carbon of PH=7 that the quartz capillary through step 3 is immersed to PH=2
In acid sodium solution, stand 3 minutes at room temperature or more, taking-up washes away residual solution with clear water；Make partial reduction graphene oxide
H is stained on film+、OH-、Na+, to complete the H of partial reduction graphene oxide+、OH-、Na+Functionalization, that is, be prepared into
Functional graphene oxide film.
Further, in the biochemical molecular solution to be measured and the mixed liquor of rhodamine liquor, rhodamine liquor it is dense
Degree is 100~300 every liter of micromoles.
The course of work of the invention are as follows: Fa-Po cavity body packaged by quartz capillary, the main sensing list as sensor
Member, when being immersed in dopamine solution, nicotine solution in the quartz capillary for having deposited functional graphene oxide film respectively
And in single stranded DNA solution and rhodamine mixed liquor, dopamine molecule, nicotine molecule and single stranded DNA and rhodamine molecule
Due to different from the adhesive capacity in functional graphene oxide, so that competitive displacement is generated, the Luo Dan in free state
Bright molecule is generated fluorescence signal by the effect of pumping laser, as the concentration dependent transducing signal of testing molecule；With DOPA
The competitive replacement result of the increase of amine molecule, nicotine molecule and single stranded DNA number, different molecules is different, sensing
Signal can also generate difference；It is encapsulated in fluorescence sense signal continuous resonance amplification in Fa-Po cavity of Fa-Po cavity body, is ultimately formed
Laser emitting；Shoot laser is linked into silicon photodetector by gold-plated single mode optical fiber completes photoelectric conversion formation fax sense letter
Number, while the reference electrical signal of another routing signal generator and the 800KHz of amplifier generation, it is mixed with electrical sensor signal access
It is mixed in frequency device, mixed electric signal will be divided into two-way, wherein access sef-adapting filter and RF analysis instrument all the way, measurement
The frequency difference of the single order beat frequency of the electric signal of its various concentration；Another way electric signal is passed through in lock-in amplifier, and the ginseng of 50KHz is arranged
Examine complete pair signals after signal locking phase amplification extract after, access in oscillograph, measure the signal that its molecule directly acts on generation
The variation of intensity.
From working principle, since dopamine molecule and the adhesive capacity of graphene oxide film are unrelated with PH,
PH can effectively displace the rhodamine molecule being adhered on graphene oxide originally in the environment of being equal to 8 and 2, and in Na+'s
It is very poor with the adhesive capacity of graphene oxide under environment, it cannot achieve the displacement with rhodamine molecule, to cannot achieve sieve
The fluorescence reproduction of red bright molecule；Due to adhesion energy of nicotine molecule in the environment of PH is equal to 8, with graphene oxide film
Power is most strong, can effectively displace the rhodamine molecule being adhered on graphene oxide originally, and is equal to 2 and Na in PH+Ring
It is very poor with the adhesive capacity of graphene oxide under border, it cannot achieve the displacement with rhodamine molecule, to cannot achieve Luo Dan
The fluorescence of bright molecule reappears；Since single strand dna is in Na+It is most strong with the adhesive capacity of graphene oxide film under environment,
The rhodamine molecule being adhered on graphene oxide originally can be effectively displaced, and in the environment of PH is equal to 8 and 2, with
The adhesive capacity of graphene oxide is very poor, cannot achieve the displacement with rhodamine molecule, to cannot achieve rhodamine molecule
Fluorescence reproduction.It can be seen that having it to dopamine point by the functionalization of the above-mentioned graphene oxide to partial reduction
Son, nicotine molecule and single strand dna are respectively provided with the ability selectively sensed.
To sum up, the beneficial effects of the present invention are:
The present invention uses mature and stable optical microcavity sensing principle, the advanced work sensed in conjunction with light optical sensing and microcavity
Skill, the integrated functionality graphene oxide film in quartz capillary aoxidize stone by functionalization as the dielectric material of sensing
The fluorescence resonance transfer characteristic of black alkene and advanced heterodyne detection and phase lock amplifying technology realize extraneous biochemical point of functionalized sensing
While sub-, the sensing sensitivity of biochemical sensor is greatly improved, sensing sensitivity can reach unimolecule magnitude；Meanwhile
The biochemical sensor is highly reliable, resists that anti-interference, signal-to-noise ratio is high, which can be directly integrated in all optical fiber system, realizes
The array detection of biochemical sensitive.
Detailed description of the invention
Fig. 1 is the selectively super quick biochemical sensor tomograph of full optical fiber laser type of the present invention.
Fig. 2 is the preparation flow figure of functional graphene oxide quartz capillary of the invention.
Fig. 3 is that selectivity of the invention senses dopamine, nicotine, single stranded DNA spectrogram.
Fig. 4 is the single molecule sensitivity schematic diagram measured of the invention.
Fig. 5 is using sensor-based system figure of the invention.
Specific embodiment
Below in conjunction with accompanying drawings and embodiments, the invention will be further described.
The selectively super quick biochemical sensitive of the full optical fiber laser type based on functional graphene oxide that the present embodiment provides a kind of
Device, structure is as shown in Figure 1, Fa-Po cavity structure includes quartz capillary, functional graphene oxide film, gold-plated single mode optical fiber
Etc. structures；Wherein:
The quartz capillary internal diameter is 126 microns, length is 1.5 centimetres, by intracavitary equally distributed oxidation
Graphene dispersing solution dry-restore-dry and etc. the reduction of inner wall deposition fraction graphene oxide film, specifically
Step are as follows:
1) clean quartz capillary is dipped vertically into the graphene oxide dispersion of 1g/L, is inhaled using capillarity
Take graphene oxide dispersion；
2) quartz capillary for having graphene oxide dispersion will be inhaled to be placed on drying station and dry, it will be quartzy after the completion of drying
Capillary, which immerses in the VC solution of 30g/L, keeps 80 DEG C of temperature water bath to heat 30 minutes, and reduction process makes graphene oxide
Become the graphene oxide of partial reduction after VC is restored；
3) it is cleaned that quartz capillary is placed on drying station again after remaining VC solution in quartz capillary with clear water and be dried
It is dry, obtain the quartz capillary that inner wall is attached with partial reduction graphene oxide film；
Above-mentioned quartz capillary is subjected to ion functionalization, specific steps later are as follows:
The quartz capillary prepared by above-mentioned requirements is subjected to functionalization in a manner of three kinds respectively: immersing the nitric acid of PH=2
In the sodium carbonate liquor of solution, the ammonium hydroxide of PH=8 and PH=7, H+、OH-、Na+With the change on the graphene oxide of partial reduction
It learns key to combine, makes to be stained with H on the graphene oxide of partial reduction respectively+、OH-、Na+, to complete the oxidation of partial reduction
The H of graphene+、OH-、Na+Functionalization, at room temperature stand 5 minutes, taking-up washes away residual solution with clear water, obtains three kinds of function
Quartz capillary can be changed, as shown in Figure 2.
Quartz capillary based on functionalization carries out selective measurement, specific steps are as follows:
The quartz capillary of functionalization in different ways is immersed into the dopamine, 20 that concentration is 10 mMs every liter respectively
Milligrams per liter nicotine, 100 every liter of nanomoles single stranded DNA and concentration be every liter of rhodamine mixed liquor of 100 micromole in it is quiet
It sets 5 minutes；Since different testing molecules are different from the competitiveness of rhodamine molecule in the quartz capillary of different function,
Through H+、OH-Fluorescence reproduction can occur when detection senses dopamine molecule for the partial reduction graphene oxide of functionalization；Through OH-Function
Fluorescence reproduction can occur when detection senses nicotine molecule for the partial reduction graphene oxide of energyization；Through Na+The portion of functionalization
Divide redox graphene that fluorescence reproduction can occur when detecting single strand dna；The quartz capillary of different function can produce
The fluorescence reproduction of raw varying strength, to achieve the purpose that selectively to sense, therefore, when wavelength is 514 nanometers of laser irradiation
When on quartz capillary, by fluorescence resonance energy transfer characteristic, unadsorbed rhodamine molecule, which generates fluorescence signal, to be led to
Spectrometer (7) is crossed to be detected, by the record analysis to fluorescence intensity, the available selection result to different molecular, choosing
It is as shown in Figure 3 that selecting property senses dopamine, nicotine, the spectrogram of single stranded DNA.
Then cavity is packaged, the structure chart after the completion of encapsulating is as shown in Figure 1, specific steps are as follows:
It is the gold that 125 nanometers 1 one end of gold-plated single mode optical fiber deposits with ion sputtering process upper one layer of 30 nanometer thickness by diameter
Film 3, the hysteroscope as Fa-Po cavity；The quartz capillary 2 of functionalization is drawn to the determinand and rhodamine of various concentration respectively
Then gold-plated single mode optical fiber is placed in quartz capillary both ends by mixed liquor, with mode of the plated film end face in, be inserted into quartzy capillary
Guan Zhong reserves one long 8 millimeters of gap 4 therebetween and stores mixed liquor.
Hereafter, based on heterodyne detection and phase lock amplifying technology, sensitivity measure is carried out, sensor-based system will be as shown in figure 5, will go out
The laser irradiation that a length of 514 nanometers of the laser 5 of ejected wave emits is when on sensor 6, since determinand molecule is easier to and quartz
The functional graphene oxide of the partial reduction of capillary tube inner wall deposition combines, therefore rhodamine molecule will not be adhered to function
Change on graphene oxide and be in free state, due to the effect of pumping laser, rhodamine molecule generates fluorescence signal, in method amber
It is intracavitary to occur to generate laser emitting after multiple resonance gain amplifies, it is linked into silicon photodetector 8 by gold-plated single mode optical fiber
It completes photoelectric conversion and forms electrical sensor signal, while the ginseng of another routing signal generator 9 and the 800KHz of the generation of amplifier 10
Electric signal is examined, accesses in frequency mixer 11 and is mixed with electrical sensor signal, mixed electric signal will be divided into two-way, wherein accessing all the way
Sef-adapting filter 12 and RF analysis instrument 13, measure the frequency difference of the single order beat frequency of the electric signal of its various concentration；Another way electricity
Signal is passed through in lock-in amplifier 15, be arranged complete pair signals after the reference signal 14 of 50KHz locking phase amplification extract after, access
In oscillograph 16, the variation that its molecule directly acts on the signal strength of generation is measured, measurement result is as shown in Figure 4；As seen from the figure,
Disengaging or absorption behavior of dopamine, nicotine and the single strand dna of different number on graphene oxide generate intensity
Different ladder-like signals.
The above description is merely a specific embodiment, any feature disclosed in this specification, except non-specifically
Narration, can be replaced by other alternative features that are equivalent or have similar purpose；Disclosed all features or all sides
Method or in the process the step of, other than mutually exclusive feature and/or step, can be combined in any way.
Claims (6)
1. a kind of selectively super quick biochemical sensor of full optical fiber laser type, comprising: 1 quartz capillary and 2 single mode optical fibers；Its
It is characterized in that, the inner wall of the quartz capillary is attached with functional graphene oxide film；The one of the every single mode optical fiber
Golden film is deposited on the end face of end, 2 single mode optical fibers are plugged in the quartz capillary with mode of the golden film end face in, are common
Mechanics amber cavity configuration；The functional graphene oxide film is by partial reduction graphene oxide film surface adhesion H+、OH-
Or Na+It is formed after ion.
2. by the selectively super quick biochemical sensor of full optical fiber laser type described in claim 1, which is characterized in that the Fa-Po cavity knot
The cavity of structure is used to store the mixed liquor of biochemical molecular solution and rhodamine liquor to be measured, the gold of mixed liquor and both ends single mode optical fiber
Film end face mechanics amber microcavity, Q value >=500,000 of the method amber microcavity.
3. by the selectively super quick biochemical sensor of full optical fiber laser type described in claim 1, which is characterized in that the Fa-Po cavity knot
The cavity length of structure is 5~8 millimeters.
4. by the selectively super quick biochemical sensor of full optical fiber laser type described in claim 1, which is characterized in that the thickness of the golden film
>=30 nanometers of degree, in reflectivity >=80% of visible light wave range.
5. by the selectively super quick biochemical sensor of full optical fiber laser type described in claim 1, which is characterized in that the functionalization oxygen
The preparation method of graphite alkene film, comprising the following steps:
Quartz capillary is dipped vertically into the graphene oxide dispersion of 0.5~3g/L by step 1, is inhaled using capillarity
Take graphene oxide dispersion；
Step 2 will inhale the quartz capillary drying for having graphene oxide dispersion, and quartz capillary is immersed 20 after the completion of drying
Temperature water bath's heating 20 minutes or more of 60~80 DEG C are kept in the VC solution of~50g/L, reduction process makes graphene oxide
Become partial reduction graphene oxide after VC is restored；
Step 3 is cleaned in quartz capillary with clear water and again dries quartz capillary after remaining VC solution, and it is attached to obtain inner wall
Have the quartz capillary of partial reduction graphene oxide film；
Step 4, nitric acid solution, the ammonium hydroxide of PH=8 or the sodium carbonate of PH=7 that the quartz capillary through step 3 is immersed to PH=2
In solution, stand 3 minutes at room temperature or more, taking-up washes away residual solution with clear water, and it is thin to be prepared into functional graphene oxide
Film.
6. by the selectively super quick biochemical sensor of full optical fiber laser type described in claim 2, which is characterized in that the biochemistry to be measured
In molecular solution and the mixed liquor of rhodamine liquor, the concentration of rhodamine liquor is 100~300 every liter of micromoles.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111190010A (en) * | 2020-01-15 | 2020-05-22 | 电子科技大学 | Micro-flow biochemical sensor in Brillouin optical machine cavity |
| CN112557349A (en) * | 2020-11-17 | 2021-03-26 | 华东师范大学重庆研究院 | SARS-CoV-2 real time in vitro fast detecting system based on graphene oxide coated microfiber sensor |
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| BAICHENG YAO: "Graphene-Enhanced Brillouin Optomechanical Microresonator for Ultrasensitive Gas Detection", 《NANO LETTERS》 * |
| MIGUEL HERNAEZ: "Optical Fibre Sensors Using Graphene-Based Materials: A Review", 《SENSORS》 * |
| SHOU-HENG LIU: "Adsorption of nicotine in aqueous solution by a defective graphene oxide", 《SCIENCE OF THE TOTAL ENVIRONMENT》 * |
| 姚佰承: "光纤/石墨烯复合光波导特性研究与器件实现", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 钱祥忠: "液晶填充 F-P 腔高精度温度传感器的研究", 《半导体光电》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111190010A (en) * | 2020-01-15 | 2020-05-22 | 电子科技大学 | Micro-flow biochemical sensor in Brillouin optical machine cavity |
| CN111190010B (en) * | 2020-01-15 | 2022-05-03 | 电子科技大学 | Brillouin optical machine intracavity microflow biochemical sensor |
| CN112557349A (en) * | 2020-11-17 | 2021-03-26 | 华东师范大学重庆研究院 | SARS-CoV-2 real time in vitro fast detecting system based on graphene oxide coated microfiber sensor |
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| CN109900667B (en) | 2021-08-06 |
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Inventor after: Yao Baicheng Inventor after: Qin Chenye Inventor after: Cao Zhongxu Inventor after: Guo Yanhong Inventor after: Rao Yunjiang Inventor before: Cao Zhongxu Inventor before: Yao Baicheng Inventor before: Qin Chenye Inventor before: Guo Yanhong Inventor before: Rao Yunjiang |