CN104877667B - A kind of fluorescence response thin-film material with humidity sensitivity and preparation method thereof - Google Patents
A kind of fluorescence response thin-film material with humidity sensitivity and preparation method thereof Download PDFInfo
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- CN104877667B CN104877667B CN201510150565.2A CN201510150565A CN104877667B CN 104877667 B CN104877667 B CN 104877667B CN 201510150565 A CN201510150565 A CN 201510150565A CN 104877667 B CN104877667 B CN 104877667B
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Abstract
The invention discloses a kind of fluorescence response thin-film material with humidity sensitivity belonging to optical sensing Material Field and preparation method thereof.The present invention is prepared for a class novel fluorescence thin-film material based on method of electrostatic spinning by compound to 4 (4 (dimethylamino) styryl) pyridine and polyvinyl pyrrolidone polymers.Simple 4 (4 (dimethylamino) styryl) pyridine does not has wet sensitive fluorescence color shifting properties, be there is the polymer of peptizaiton by introducing, change space arrangement mode and the intermolecular interaction of 4 (4 (dimethylamino) styryl) pyridine organic molecule, cause different extraneous relative humidity can change rapidly the fluorescence property of 4 (4 (dimethylamino) styryl) pyridine and polymer composite film.This composite takes full advantage of electrostatic spinning technique can be prepared and have polymolecularity and the feature of high-ratio surface film, short for the wet sensitive fluorescence sense device and response time with high-quality optical characteristics, the most hygroscopic manufacture and design provide new approach.
Description
Technical field
The invention belongs to optical sensing field of material technology, in particular, provide one and there is humidity
Fluorescence response thin-film material of sensitivity characteristic and preparation method thereof.For novel fluorescence sense film material
Material preparation provides new mentality of designing and feasible scheme.
Background technology
Humidity is extraneous factor important in environment for human survival, and relative humidity generally represents air
The percentage of middle contained humidity.Efficient and the fast monitored of humidity is for environmental protection, meteorological, aviation,
Food, light industry, chemicals, the numerous areas such as pharmacy is significant.Currently, common
Humidity sensor (such as hygrometer) is electronics principle based on semiconductor element.By the external world
The change of humidity causes the electrology characteristic (such as resistance, electric capacity and dielectric constant etc.) of semiconductor element
Change, thus realize the monitoring to humidity.But current hygrometer exists humidity sound
Between Ying Shi, how the problem such as longer, Humidity Detection hysteresis quality, develop novel fast response time,
The humidity sensitive material that resolution ratio is high is the developing direction of following intellectualized detection,
Fluorescence analysis has the response feature such as sensitive and readily identified.In recent years, intelligent response is glimmering
Luminescent material has had tremendous development, and such material refers in the different extraneous thorns such as optical, electrical, pressure, heat
Under Jiing, thus it is possible to vary the transmitting wavelength of fluorescence.Due to spies such as its signal are sensitive, fast response time
Point, increasingly gets more and more people's extensive concerning, and this kind of material is at sensor, optical anti-counterfeiting and opens
The fields such as pass have extremely strong using value.How based on above-mentioned intelligent response principle Development of Novel
Humidity sensitive fluorescent material be build Novel humidity sensing element Critical policies.At present, tool
The fluorescent material having Rapid reversible monitoring humidity change also rarely has report.Meanwhile, in order to meet not
Carry out the realization of humidity fluorescent device and sensing function, prepare humidity by simple and effective method quick
Sense fluorescence membrane material remains a challenge.
Electrostatic spinning is a kind of to prepare the simple, with low cost of nano-micrometre yardstick fiber
Effective way.This technology is by polymer or to have viscoelastic solution system by high-pressure electrostatic
Standby become micron or nanometer grade diameter fiber until a kind of process technology of fiber membrane.Electrostatic spinning
Fiber membrane is because having high-specific surface area, the feature such as easily operated and carrying at medicine and release, ultra-clean receive
The aspects such as rice filtration, water process, cosmetics and the energy have higher using value.Pass through electrostatic
The film that spining technology obtains is unordered on meso-scale, but in macroscopically its physical property is again
Uniformly.The optical property of the fluorescence membrane therefore obtained by method of electrostatic spinning has good equal
One property.Prepare simplicity and the designability of film based on electrostatic spinning, be expected to by this kind of side
Method obtains the novel optical material with special optical performance.
The present invention combines closely the growth requirement of current humidity sensitive material, rings in combination with intelligence
The problem answering the aspects such as fluorescent material response effect to exist, chooses (4-(4-(dimethylamino) styrene
Base) pyridine compounds as prepare humidity sensitive response film molecule primitive, by polyvinyl pyrrole
Alkanone, as the medium molecule of formation thin-film material, is prepared by method of electrostatic spinning and is had humidity
The Intelligent fluorescent thin-film material of response.By modulation (4-(4-(dimethylamino) styryl) pyridine
Compound and the mass ratio of polyvinylpyrrolidone, it is achieved that the tune of material wet sensitive fluorescence color changeable effect
Control.Compared to respond without humidity simple (4-(4-(dimethylamino) styryl) pyridine compounds,
Series film material achieves material stimulates the characteristic of fluorescence response to humidity.And the method has
Have easy and simple to handle, with low cost and sensitivity advantages of higher.
Summary of the invention
Object of the present invention is to provide a kind of fluorescence response film with humidity sensitivity
Material and preparation method thereof, the design synthesis for Development of Novel humidity response fluorescence membrane provides new
Thinking and method.
The present invention is by by (4-(4-(dimethylamino) styryl) pyridine compounds and polyvinyl pyrrole
Alkanone mixed solution is prepared for novel fluorescence thin-film material by method of electrostatic spinning.(4-(4-(diformazan ammonia
Base) styryl) the pyridine compounds characteristic that wet sensitive does not responds itself；Have point when introducing
Dissipate the polymer of effect, change space arrangement mode and the intermolecular interaction of organic molecule,
Thin-film material is made to have rapidly, reversible humidity response optical property.This composite is abundant
Make use of electrostatic spinning to prepare high dispersive and the feature of high-ratio surface film, obtained that there is humidity
The novel fluorescence thin-film material of stimuli responsive characteristic, for having the intelligent sensing of high-quality optical characteristics
The preparation of material and optical anti-counterfeiting device provides new thinking and approach.
Preparation process is as follows:
1) preparation of electrostatic spinning solution:
A. the amount weighing material is 1 × 10-4～5 × 10-44-(4-(dimethylamino) styryl) pyridine of mol
(being called for short DSP).
B. weighing PVP K90 (being called for short PVP), the amount of its material is 3 × 10-6~
6×10-6mol；
C. above-mentioned DSP Yu PVP is dissolved in the methanol solution of 10～30ml jointly.
D. the solution that DSP with PVP is blended is stirred until powder is completely dissolved.
2) preparation of fluorescence membrane:
A. the preparation of electrostatic spinning instrument: syringe needle and the receiving range collected between screen are regulated
It is 10～25cm；Relative humidity 30% in instrument；Temperature 60 C；Select the pin of spinning nozzle
Head shapes is round.
B. the methanol solution that DSP Yu PVP is blended is added in spray nozzle device；
C. applying the high voltage of 20～30KV, solution is changed into band electrojet under high-tension effect
Stream, described injection stream is deposited on the surface of receiving screen；
D., after the electrostatic spinning of certain time, receiving screen is collected one layer of uniform white fine
Dimension film ultimately forms size and is about 30cm × 40cm film.
By above-mentioned prepared material:
1. put in any atmosphere that relative humidity is 15% to 95%, the fluorescence of film be can be observed
Blue-green or green is become from blueness.
2. carry out fluorescence spectrum to characterize the emission spectrum of display film and there occurs bright along with the increase of humidity
Aobvious red shift.
It is an advantage of the current invention that: by (4-(4-(dimethylamino) styryl) pyridine compounds is with poly-
Vinylpyrrolidone mixed solution is prepared for novel wet sensitive fluorescence response film by method of electrostatic spinning
Material.And single (4-(4-(dimethylamino) styryl) pyridine compounds itself there is no this characteristic.
Electrostatic spinning process can realize that (4-(4-(dimethylamino) styryl) pyridine compounds is at polymer
High degree of dispersion in matrix, thus change the space arrangement mode of molecule and intermolecular phase interaction
With so that regulate and control rapidly (4-(4-(dimethylamino) styryl) pyridine by the change of ambient humidity
The fluorescence property of compound.This composite takes full advantage of electrostatic spinning, and to prepare high-ratio surface thin
The feature of film, has obtained the novel fluorescence thin-film material with humidity stimuli responsive, it is achieved that
(optimization of 4-(4-(dimethylamino) styryl) pyridine compounds optical function and change, widen
The application space of single compound film and preparation scope.Simultaneously for have high-quality optical characteristics
The preparation of novel intelligent material and optical anti-counterfeiting material provides new thinking and approach.
Accompanying drawing explanation
Fig. 1 is that DSP@PVP (0.5%) film humidity responds fluorogram
Fig. 2 is that DSP@PVP (1.0%) film humidity responds fluorogram
Detailed description of the invention
[embodiment 1]
1) 0.0265g (4-(4-(dimethylamino) styryl) pyridine chemical combination is weighed
Thing DSP, and 5.3g polyvinylpyrrolidone PVP；
2) both are mixed, put in 15ml methanol solution, at 20ml
In beaker, to stir two hours under the conditions of 3000r/min；
3) preparation of fluorescence membrane:
A. the preparation of electrostatic spinning instrument: syringe needle and the distance collected between screen are regulated
For 17cm；Instrument humidity is 30%；Temperature is 50 DEG C；Select the syringe needle shape of spinning nozzle
Shape is round；
B. the methanol solution containing DSP and PVP is added in spray nozzle device；
C. applying the high voltage of 22KV, solution is changed into band electrojet under high-tension effect
Stream, described injection stream is deposited on the surface of base material；
D. the polymer and in described injection stream solidifies thus forms nanofiber, ultimately forms certainly
It it is so the film of white under light.
[embodiment 2]
1) weigh 0.0530g (4-(4-(dimethylamino) styryl) pyridine compounds DSP, and
5.3g polyvinylpyrrolidone PVP；
2) both are mixed, put in 25ml methanol solution, in 50ml beaker,
To stir two hours under the conditions of 2000r/min；
3) preparation of fluorescence membrane:
A. the preparation of electrostatic spinning instrument: syringe needle and the distance collected between screen are regulated
For 17cm；Instrument humidity is 25%；Temperature is 50 DEG C；Select the syringe needle shape of spinning nozzle
Shape is round；
B. the methanol solution containing DSP and PVP is added in spray nozzle device；
C. applying the high voltage of 22KV, solution is changed into band electrojet under high-tension effect
Stream, described injection stream is deposited on the surface of base material；
D. the polymer and in described injection stream solidifies thus forms nanofiber, ultimately forms certainly
It it is so the film of white under light.
Product in embodiment 1 and example 2 is characterized: the film of different humidity is carried out glimmering
Optical tests, film emission spectrum under conditions of humidity increases occurs the reddest as seen from the figure
Move.
Claims (2)
1. a fluorescence response thin-film material with humidity sensitivity, it is characterised in that based on quiet
Electrospinning, described material 4-(4-(dimethylamino) styryl) pyridine and polyethylene pyrrole
Pyrrolidone is mixed with fluorescence membrane, thus changes 4-(4-(dimethylamino) styryl) pyridine
The space arrangement of organic molecule and interaction mode, the loose and high-ratio surface of film is special simultaneously
Property make regulate and control rapidly 4-(4-(dimethylamino) styryl) pyridine by different extraneous relative humidity
Fluorescence property with polymer composite film.
2. having a preparation method for the fluorescence response thin-film material of humidity sensitivity, its feature exists
In, its concrete operation step is as follows:
1) preparation of electrostatic spinning solution:
A. the amount weighing material is 1 × 10-4～5 × 10-44-(4-(dimethylamino) styryl) pyridine of mol,
It is called for short DSP；
B. weighing PVP K90, referred to as PVP, the amount of its material is 3 × 10-6~
6×10-6mol；
C. above-mentioned DSP Yu PVP is dissolved in the methanol solution of 10～30mL jointly；
D. the solution that DSP with PVP is blended is stirred until powder is completely dissolved；
2) preparation of fluorescence membrane:
A. the preparation of electrostatic spinning instrument: syringe needle and the receiving range collected between screen are regulated
It is 10～25cm；Relative humidity 30% in instrument；Temperature 60 C；Select the pin of spinning nozzle
Head shapes is round；
B. the methanol solution that DSP Yu PVP is blended is added in spray nozzle device；
C. applying the high voltage of 20～30KV, solution is changed into band electrojet under high-tension effect
Stream, described injection stream is deposited on the surface of receiving screen；
D., after the electrostatic spinning of certain time, receiving screen is collected one layer of uniform white fine
Dimension film, ultimately forms size and is about 30cm × 40cm film.
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| CN106539696B (en) * | 2016-12-07 | 2019-07-23 | 江南大学 | The application of 5-ALA |
| CN107268182B (en) * | 2017-05-18 | 2019-08-20 | 武汉纺织大学 | To the nano micro crystal cellulose nano-fiber composite film and preparation method thereof of humidity sensitive |
| CN109280305B (en) * | 2017-07-21 | 2021-06-08 | 香港科技大学 | Preparation and application of humidity visualization material with aggregation-induced emission characteristic |
| CN111410790B (en) * | 2020-04-29 | 2022-10-25 | 广东圆融新材料有限公司 | Humidity-sensitive fluorescent modified polypropylene material and preparation method thereof |
| CN114773492B (en) * | 2022-05-13 | 2023-03-07 | 井冈山大学 | Starch-based composite material, preparation method and application thereof, starch-based organic film, and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6086920A (en) * | 1998-08-12 | 2000-07-11 | Fuisz Technologies Ltd. | Disintegratable microspheres |
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2015
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6086920A (en) * | 1998-08-12 | 2000-07-11 | Fuisz Technologies Ltd. | Disintegratable microspheres |
Non-Patent Citations (3)
| Title |
|---|
| Effect of moisture on polyvinylpyrrolidone in accelerated stability testing;Shaun Fitzpatrick et al.;《International Journal of Pharmaceutics》;20021231;第246卷;143-151 * |
| Fibre-optic sensor technologies for humidity and moisture measurement;T.L. Yeo et al.;《Sensors and Actuators A》;20080206;第122卷;280-295 * |
| Humidity sensing with a luminescent Ru(II) complex and phase-sensitive detection;Maximino Bedoya et al.;《Sensors and Actuators B》;20050810;第113卷;573-581 * |
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