CN106353257A - Amino-functionalization photonic crystal thin film sensor for visual detection of volatile aldehyde - Google Patents
Amino-functionalization photonic crystal thin film sensor for visual detection of volatile aldehyde Download PDFInfo
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- CN106353257A CN106353257A CN201510424316.8A CN201510424316A CN106353257A CN 106353257 A CN106353257 A CN 106353257A CN 201510424316 A CN201510424316 A CN 201510424316A CN 106353257 A CN106353257 A CN 106353257A
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Abstract
The invention relates to a preparation method of an amino-functionalization photonic crystal thin film sensor for visual detection of volatile aldehyde. The preparation method comprises the following specific steps: modifying amino on a reverse opal photonic crystal thin film through spin-coating of an amino-containing polymer or under the action of a chemical bond, changing the average refractive index of a sensing thin film by using reversible reaction of the amino and a formyl group and a three-dimensional macroporous structure of a reverse opal photonic crystal through the reversible chemical and physical action of the sensing thin film to volatile aldehyde gas so as to enable a reflection spectrum to move, and selecting the proper photonic crystal to enable the reflection spectrum to move within a visible light range to finally cause a change of the color of the thin film. Therefore, high-sensitivity and reversible visual detection for the volatile aldehyde gas is realized.
Description
Technical field
The present invention relates to volatile organic gas detection field, specifically, it is to be related to a kind of preparation method of gas sensor.
This sensing material is a kind of photon crystal film material of amino functional, effective using position of photon crystal forbidden band mobile visualization
Detect the gas of volatile aldehyde, can be used for improving the detection sensitivity of gaseous aldehyde, effectively overcome in traditional detection method simultaneously
Sensing material can only disposable defect.
Background technology
The aldehyde materials such as formaldehyde have been confirmed as carcinogenic by World Health Organization (WHO) (who) and have been caused deformed material, are also potentially strong
One of mutagenic matter.Aldehyde material is mainly manifested in heterosmia, allergy, immunologic function disorder etc. to the health effect of the mankind
Aspect.Long Term Contact low dosage formaldehyde can cause chronic respiratory tract disease.Therefore, the efficient detection to aldehydes steam, to the mankind
Life health and environment have important realistic meaning.
The method of traditional detection aldehyde material steam mainly have colorimetry (c.l.p.thomas, f.meunier, c.a.veasey,
C.d.mcgill, anal.commun.1998,35,103.), red, orange, green, blue, yellow (ROGBY) (e.r.kennedy, r.h.hill, anal.
Chem.1982,54,1739), polarogarphy (z.q.zhang, h.zhang, g.f.he, talanta2002,57,317.),
Fluorimetry (j.y.lai and, y.t.li, biomacromolecules 2010,11,1387.) and quartz crystal microbalance method
(b.ding, x.wang, j.yu, m.wang, j.mater.chem.2011,21,12784.) etc..Said method needs expensive
Main equipment, longer detection time.Optical sensing is received much concern with the feature of simple, quick, safety and on-line real-time measuremen.
The reflectance spectrum of monitoring sensing material even more the most intuitively method, especially when reflection peak is located at visible region, Ke Yishi
Existing open hole detection.
The development of photonic crystal technology in recent years, the gas sensor especially using Responsive photonic crystals as sensitive membrane is as new biography
One pith of sensor, its research and development constantly obtains new breakthrough.Its application be related to ambient humidity, soda acid atmosphere,
The detection of the various chemical substance such as environmental contaminants, is a kind of safe ready again efficiently detection meanss.Photonic crystal is a kind of Jie
The different material periodicities arrangement of electric constant, makes the light of characteristic frequency cannot pass through this crystal and can be had by strong reflection
The characteristic of forbidden photon band.When the frequency of light falls in the range of the forbidden photon band of photonic crystal, will be by strong anti-of photonic crystal
Penetrate, referred to as Bragg reflection.Sailor [a.m.ruminski, m.m.moore, m.j.sailor, adv.funct.mater.
The one-dimensional photon that two kinds of different dielectric substances 2008,18,3418.] et al. are filled in preparation in the cavernous structure of porous silicon is brilliant
Body, the efficient gas sensor not affected by air humidity, different steams are distinguished by the movement of peak frequency.Chinese section
Chemistry institute Song Yan woods seminar of institute [e.tian, j.wang, y.zheng, y.song, l.jiang, d.zhu, j.mater.
Chem.2008,18,1116.] fill imbibition thing polyacrylamide in polymerase proteins stone-type photonic crystal gap, when outer
When boundary's humidity changes, polyacrylamide water suction expands, thus leading to the forbidden photon band of photonic crystal that red shift occurs, real
Show the colour sensing to humidity.Gu Zhongze seminar of Southeast China University [z.xie, k.cao, y.zhao, l.bai, h.gu, h.xu,
Z.-z.gu, adv.mater.2014,26,2413.] using surface-functionalized mesoporous sio2Colloidal crystal bead is to gas with various
Absorption, can detect multiple gases simultaneously, obtain greater advance in terms of photonic crystal detected gas.
This seminar is in tio2Polyaniline is filled, using polyaniline and nh in inverse opal photonic crystal3With taking off of hcl gas
Doping and doping acts on, and changes the refractive index of photon crystal film, and Bragg reflection peak moves, and thin film color changes, real
Visual retrieval (c.liu, g.gao, y.zhang, l.wang, j.wang, y.song, macromol. to Acid-base Gas are showed
Rapid commun.2012,33,380.).In sio2Hexaphenyl silicon base compound is filled in inverse opal photonic crystal gap, can
With Visual retrieval ether and petroleum ether gas (y.zhang, j.qiu, m.gao, p.li, l.gao, l.heng, b.z.tang,
L.jiang, j.mater.chem.c2014,2,8865), filling tetraphenyl ethylene based polyalcohol achieves to oxolane and acetone gas
Visual retrieval (y.zhang, j.qiu, r.hu, p.li, l.gao, l.heng, b.tang, l.jiang, the phys. of body
Chem.chem.phys.2015,17,9651).
At present, although photonic crystal detected gas research more, using photonic crystal reflectance spectrum mobile visualization detection
Have the detection of volatile aldehyde of serious threat there is not been reported to human health.
Content of the invention
The present invention is incorporated into the detection field of volatile aldehyde the unique optical property of photonic crystal, with polyallylamine (pah) or 3-
Aminopropyl-triethoxysilane (3-aminopropyl) triethoxysilane, be abbreviated as apts) } modify sio2Counter opal light
Sub- crystal (is abbreviated as sio2- iopc), obtain the photon crystal film of amino functional, using the reversible reaction of amino and aldehyde radical
(y.zhu, h.li, q.zheng, j.xu, x.li, langmuir2012,28,7843.), and the three of inverse opal photonic crystal
Dimension macroporous structure, by chemically and physically adsorbing the gas of volatile aldehyde, changes the mean refractive index of photon crystal film, thus
Change its reflectance spectrum, and then cause the change of thin film color, finally realize highly sensitive, the reversible visualization to volatile aldehyde
Detection.
The sio of the amino functional of the present invention2- iopc thin film sensor detects that the step of volatile aldehyde includes:
(1) preparation has the sio of different forbidden photon bands2-iopc
Polystyrene monodisperse polymer micro-sphere-sio is prepared under the conditions of constant temperature and humidity using common construction from part2Nanocomposites
Photonic crystal template, is soaked with organic solvent or the method for high temperature sintering removes polymer microballoon template, prepares
sio2- iopc, characterizes pattern and forbidden photon band with scanning electron microscope and reflectance spectrum.Regulation and control preparation parameter, preparation reflectance spectrum exists
The sio of visible region2-iopc.
(2) prepare the sio of amino functional2-iopc
The present invention includes two kinds of amination method: one is in sio2Fill pah in the hole of-iopc, spin coating can be passed through, drip
The mode applying or soaking absorption is filled;Two is sio2- iopc carries out hydrophilic treated, is then immersed in the toluene solution of apts.
Amination is carried out by surface self-organization.
(3) detection of volatile aldehyde
The sio of made amino functional2- iopc sense film is placed in the gaseous environment of volatile aldehyde, online with fiber spectrometer
The reflectance spectrum of detection photonic crystal, and the color change with photo recording sheet.Study made sensor full in volatile aldehyde
With reflectance spectrum under vapour pressure over time;Research reflectance spectrum determines detection sensitivity with the change of gas concentration;Research
In different volatile organic solvent steams, the change of reflectance spectrum is to investigate the selectivity to volatile aldehyde gas detecting for the sensor.
(4) reusability of made sensor
The sio of made amino functional2- iopc sensor is alternately placed in gas and the air atmosphere of volatile aldehyde, uses fiber spectrum
The change of instrument on-line checking reflectance spectrum, investigates the reusability that made photon crystal film sensor detects volatile aldehyde.
In the preparation method of the present invention, the basic demand that functional molecular and photonic crystal are selected is: functional molecular carries amino,
Can interact with aldehyde radical;The forbidden photon band of photonic crystal is located in visible-range, is alternately exposed to aldehydes steam and in the air
The reflectance spectrum of photonic crystal sensors is reversible change in visible-range, and thin film color change is visually observed, thus realizing
Purpose using functionalization photon crystal film open hole detection aldehydes steam;
The present invention mainly uses the inverse opal photonic crystal of amino functional, by the chemical action and three of amino and aldehyde radical
The absorption to gas for the high-specific surface area of dimension macroporous structure, changes the mean refractive index of photon crystal film so as to reflected light spectral shift
Dynamic, thus causing the change of thin film color, finally realize highly sensitive, the reversible Visual retrieval to volatile aldehyde.
It is an advantage of the current invention that:
The present invention utilizes the reversible reaction that amino is with aldehyde radical and the high-specific surface area of inverse opal photonic crystal three-dimensional macroporous structure
Matter, from the amidized photonic crystal in visible region for the forbidden photon band, with target steam effect back reflection spectrum in visible ray
In the range of move, thin film color occur corresponding change, thus realizing bore hole monitoring, strengthen the practicality of sensor;Using ammonia
Base and the interaction of aldehyde radical, improve the selectivity of detection;Strengthen gas absorption using high-specific surface area characteristic, improve detection
Sensitivity;It is to achieve the recyclability of sensor using reversible physics, chemical action.Actually detected for toxic vapours
More convenient, quick, provide a brand-new thinking for exploitation novel thin film gas sensor.
Brief description
Accompanying drawing 1: particle diameter is the photon crystal film (a) of poly- (Styrene And Chloroalkyl Acrylates) microsphere preparation of 340nm, polymer microballoon-sio2
Colloidal sol composite photonic crystal (b) and sio2The sem photo of inverse opal photonic crystal (c);
Accompanying drawing 2: polymer microballoon-sio2(black line is labeled as p (st-aa)-sio to colloidal sol composite photonic crystal2)、sio2Anti- albumen
(green line is labeled as sio to stone photonic crystal2) and pah-sio iopc2(red line is labeled as pahsio to inverse opal photonic crystal2
Iopc reflectance spectrum);
Accompanying drawing 3:pah-sio2Iopc is exposed to reflection peak spectrum and its photo (c) in formaldehyde (a) and air (b);
Accompanying drawing 4:pah-sio2Iopc is exposed to the reflection peak spectrum in acetaldehyde (a) and air (b);
Accompanying drawing 5:pah-sio2Iopc is exposed to the reflection peak spectrum in propionic aldehyde (a) and air (b);
Accompanying drawing 6:pah-sio2Iopc is exposed to the reflection peak spectrum in butyraldehyde (a) and air (b);
Accompanying drawing 7:pah-sio2Iopc is exposed to the reflection peak spectrum in valeral (a) and air (b).
Specific embodiments
Embodiment 1
The sio of pah filling2- iopc thin film Visual retrieval formaldehyde
1.1sio2The preparation of colloidal sol
sio2Colloidal sol is with ethanol as solvent according to literature method, and concentrated hydrochloric acid (0.1m) hydrolyzes tetraethyl orthosilicate for catalyst
Prepared by (teos, 28wt.%), teos, concentrated hydrochloric acid and ethanol be in mass ratio 1: 1: 2 ratio mixing after magnetic force at room temperature
Stirring 1h, that is, obtain transparent sio2Colloidal sol.
1.2sio2The preparation of-iopc thin film
Obtained on the glass substrate using the vertical method depositing assembling altogether under conditions of constant temperature and humidity.Substrate of glass (3cm ×
1.2cm) heated and boiled 30min in the washing liquid of sulfuric acid/hydrogen peroxide (volume ratio 3: 1), wait after cooling successively use tap water,
Distilled water flushing is clean.Configuration quality percentage ratio is~0.2% polystyrene-acrylic emulsion 20g in conical flask, ultrasonic
0.1ml sio is added after 10min2Colloidal sol is further continued for ultrasonic 30min.Mixed emulsion pours the small beaker of clean 5ml into
In, clean substrate of glass is vertically placed in small beaker, film forming 48h under 65 DEG C of constant temperature, obtains polymer
Microsphere-sio2Photonic crystal laminated film.Finally, made laminated film, in 500 DEG C of calcination 4h, completely removes polymerization with guarantee
Thing microsphere, obtains sio2- iopc (2cm × 1.2cm), in purple.With scanning electron microscope, table is carried out to surface topography
Levy (accompanying drawing 1), forbidden photon band is characterized (accompanying drawing 2) with reflectance spectrum.
1.3pah-sio2The preparation of-iopc
Configuration quality percentage ratio is 0.1% pah aqueous solution, adjusts ph between 7-8 with ammonia, by the sio preparing2-iopc
Thin film is immersed 5min, takes out after drying again in 40 DEG C of dry for standby.
The detection of 1.4 formaldehyde vaporses
Made pah-sio2- iopc thin film is placed in the saturated vapor of formaldehyde, with fiber spectrometer on-line checking photonic crystal
Reflectance spectrum, such as accompanying drawing 3a, reflectance spectrum moves 129nm, and thin film color is changed into yellow green by original purple.Due to
Amino on pah and the additive reaction of formaldehyde, the macroporous structure absorbing formaldehyde gas of counter opal, make made sensor simultaneously
There is red shift in the reflectance spectrum of thin film;And when being positioned in the air, amino and the addition of formaldehyde are reversible reaction, physical absorption
Formaldehyde gases can be desorbed again, and therefore reflectance spectrum occurs blue shift again, such as accompanying drawing 3b.Work as pah-sio2- iopc thin film is alternately put
When formaldehyde gases and in the air, reflectance spectrum occur can reverse response, illustrate that made sensor is reusable.Additionally, detection
Under gas with various concentration, the change of reflectance spectrum, determines sensitivity;The response of the other gas of detection, determines selectivity.
Embodiment 2
The sio of pah filling2- iopc thin film Visual retrieval acetaldehyde
1.1sio2The preparation of colloidal sol
With embodiment 1 1.1.
1.2sio2The preparation of-iopc thin film
With embodiment 1 1.2.
1.3pah-sio2The preparation of-iopc
With embodiment 1 1.3.
The detection of 1.4 acetaldehyde steams
Made pah-sio2- iopc thin film is placed in the saturated vapor of acetaldehyde, with fiber spectrometer on-line checking reflectance spectrum,
Spectral red shift, such as accompanying drawing 4a, reflectance spectrum moves 106nm, and thin film color is changed into yellow green by original purple;And put
When being placed in the air, there is blue shift in reflectance spectrum again, such as accompanying drawing 4b.Work as pah-sio2- iopc thin film is alternately placed in acetaldehyde gas
When body and in the air, reflectance spectrum occur can reverse response, illustrate that made sensor is reusable.
Embodiment 3
The sio of pah filling2- iopc thin film Visual retrieval propionic aldehyde
1.1sio2The preparation of colloidal sol
With embodiment 1 1.1.
1.2sio2The preparation of-iopc thin film
With embodiment 1 1.2.
1.3pah-sio2The preparation of-iopc
With embodiment 1 1.3.
The detection of 1.4 propionic aldehyde steams
Made pah-sio2- iopc thin film is placed in the saturated vapor of propionic aldehyde, with fiber spectrometer on-line checking reflectance spectrum,
Spectral red shift, such as accompanying drawing 5a, reflectance spectrum moves 108nm, and thin film color is changed into yellow green by original purple;And put
When being placed in the air, there is blue shift in reflectance spectrum again, such as accompanying drawing 5b.Work as pah-sio2- iopc thin film is alternately placed in acetaldehyde gas
When body and in the air, reflectance spectrum occur can reverse response, illustrate that made sensor is reusable.
Embodiment 4
The sio of pah filling2- iopc thin film Visual retrieval butyraldehyde
1.1sio2The preparation of colloidal sol
With embodiment 1 1.1.
1.2sio2The preparation of-iopc thin film
With embodiment 1 1.2.
1.3pah-sio2The preparation of-iopc
With embodiment 1 1.3.
The detection of 1.4 butyraldehyde steams
Made pah-sio2- iopc thin film is placed in the saturated vapor of butyraldehyde, with fiber spectrometer on-line checking reflectance spectrum,
Spectral red shift, such as accompanying drawing 6a, reflectance spectrum moves 134nm, and thin film color is changed into redness by original purple;And place
When in the air, there is blue shift in reflectance spectrum again, such as accompanying drawing 6b.Work as pah-sio2- iopc thin film is alternately placed in aldehydes gas
During with the air, reflectance spectrum occur can reverse response, illustrate that made sensor is reusable.
Embodiment 5
The sio of pah filling2- iopc thin film Visual retrieval valeral
1.1sio2The preparation of colloidal sol
With embodiment 1 1.1.
1.2sio2The preparation of-iopc thin film
With embodiment 1 1.2.
1.3pah-sio2The preparation of-iopc
With embodiment 1 1.3.
The detection of 1.4 valeral steams
Made pah-sio2- iopc thin film is placed in the saturated vapor of valeral, with fiber spectrometer on-line checking reflectance spectrum,
Spectral red shift, such as accompanying drawing 7a, reflectance spectrum moves 115nm, and thin film color is changed into yellow green by original purple;And put
When being placed in the air, there is blue shift in reflectance spectrum again, such as accompanying drawing 7b.Work as pah-sio2- iopc thin film is alternately placed in acetaldehyde gas
When body and in the air, reflectance spectrum occur can reverse response, illustrate that made sensor is reusable.
Embodiment 6
The sio that apts modifies2The volatile aldehyde of-iopc thin film Visual retrieval
1.1sio2The preparation of colloidal sol
With embodiment 1 1.1.
1.2sio2The preparation of-iopc thin film
Obtained on the glass substrate using the vertical method depositing assembling altogether under conditions of constant temperature and humidity.Substrate of glass (3cm ×
1.2cm) heated and boiled 30min in the washing liquid of sulfuric acid/hydrogen peroxide (volume ratio 3: 1), wait after cooling successively use tap water,
Distilled water flushing is clean.Configuration quality percentage ratio is~0.2% polystyrene emulsion 20g in conical flask, after ultrasonic 10min
Add 0.1ml sio2Colloidal sol is further continued for ultrasonic 30min.Mixed emulsion is poured in the small beaker of clean 5ml, will do
Net substrate of glass is vertically placed in small beaker, film forming 48h under 65 DEG C of constant temperature, obtains polymer microballoon-sio2
Photonic crystal laminated film.Finally, made laminated film, in 500 DEG C of calcination 4h, completely removes polymer microballoon with guarantee,
Obtain sio2-iopc(2cm×1.2cm).
1.3apts-sio2The preparation of-iopc
Configuration concentration is the toluene solution of the apts of 1-10%, by made sio2- iopc thin film is immersed certain time.
The detection of 1.4 volatile aldehyde
Made apts-sio2- iopc thin film is respectively placed in the saturation of the volatile aldehyde such as formaldehyde, acetaldehyde, propionic aldehyde, butyraldehyde, valeral
In steam, with fiber spectrometer on-line checking reflectance spectrum, spectrum generation red shift;When being then positioned in the air again, reflected light
There is blue shift b in spectrum again.Work as apts-sio2When-iopc thin film is alternately placed in gas and the in the air of volatile aldehyde, reflectance spectrum
Generation can reverse response, illustrate that made sensor is reusable.
Claims (3)
1. a kind of amino functional photon crystal film sensor visualization detect volatile aldehyde preparation method it is characterised in that: with
The inverse opal photonic crystal of amino functional is sense film, and the functional molecular load specially containing amino or modification are in photon
On crystal, the polymer that amino can be contained by spin coating or amino is modified by chemical bond.Change reversible to amino and aldehyde radical
Learning reaction is conducive to the characteristic of adsorbed gas to combine with counter opal three-dimensional macroporous structure, by sense film to object gas
Reversible chemically and physically effect, changes the mean refractive index of sense film, so that reflectance spectrum is moved and selects properly
Photonic crystal so that reflectance spectrum is moved in visible-range, finally cause the change of thin film color, realize to volatile aldehyde gas
The Visual retrieval of body.
2. a kind of amino functional photon crystal film sensor visualization detect volatile aldehyde preparation method it is characterised in that: choosing
Take forbidden photon band in the sio of visible region2Fill polyallylamine in inverse opal photonic crystal, then its hole, using amino and
Aldehyde radical reversible chemical reaction and the characteristic of counter opal three-dimensional macroporous structure adsorbed gas, realize the visualization inspection to volatile aldehyde
Survey.
3. a kind of amino functional photon crystal film sensor visualization detect volatile aldehyde preparation method it is characterised in that: choosing
Take forbidden photon band in the sio of visible region2Inverse opal photonic crystal, assembles 3- aminopropyl-three ethoxy by self-assembling method
Base silane, using the characteristic of amino and aldehyde radical reversible chemical reaction and counter opal three-dimensional macroporous structure adsorbed gas, it is right to realize
The Visual retrieval of volatile aldehyde.
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CN108226115A (en) * | 2017-12-29 | 2018-06-29 | 华南师范大学 | It is a kind of to be used for formaldehyde gas, the nano combined sensitive membrane of humidity and the multi-functional detection of temperature and its preparation |
CN110836858A (en) * | 2019-12-05 | 2020-02-25 | 中国科学院化学研究所 | Method for nondestructive real-time detection of chemical reaction process based on photonic crystal |
CN113213488A (en) * | 2021-05-07 | 2021-08-06 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Aptamer inverse opal photonic crystal sensing material and method for rapidly and ultrasensitively detecting staphylococcus aureus enterotoxin B without markers |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108226115A (en) * | 2017-12-29 | 2018-06-29 | 华南师范大学 | It is a kind of to be used for formaldehyde gas, the nano combined sensitive membrane of humidity and the multi-functional detection of temperature and its preparation |
CN108226115B (en) * | 2017-12-29 | 2020-09-08 | 华南师范大学 | Nano composite sensitive membrane for multifunctional detection of formaldehyde gas, humidity and temperature and preparation thereof |
CN110836858A (en) * | 2019-12-05 | 2020-02-25 | 中国科学院化学研究所 | Method for nondestructive real-time detection of chemical reaction process based on photonic crystal |
CN113213488A (en) * | 2021-05-07 | 2021-08-06 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Aptamer inverse opal photonic crystal sensing material and method for rapidly and ultrasensitively detecting staphylococcus aureus enterotoxin B without markers |
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