CN104961906B - A kind of photonic crystal hydrogel thin film, its preparation method and application for having pH value and ionic strength response concurrently - Google Patents
A kind of photonic crystal hydrogel thin film, its preparation method and application for having pH value and ionic strength response concurrently Download PDFInfo
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Abstract
The invention discloses a kind of photonic crystal hydrogel thin film, its preparation method and application for having pH value and ionic strength response concurrently.The photonic crystal hydrogel thin film includes Fe3O4Nano-particle and polyacrylamide metering system acid hydrogel；The Fe3O4Nano-particle is dispersed in hydrogel, is arranged in one-dimensional chain, and the concentration of nano-particle in the film is 1~50mg/mL.The preparation method of described photonic crystal hydrogel thin film, including by Fe3O4Nano-particle and hydrogel monomer uniformly mix, and bring it about curing reaction by ultraviolet light, are finally dipped in the soluble carbonate salt aqueous solution, so as to obtain required film.The preparation method of the present invention is simple to operate, and repeatability is strong, is easy to prepare on a large scale, and obtained film carboxyl amount is controllable, and film is in monochrome, and pH value or ionic strength have obvious color change under stimulating, be suitable for open hole detection.
Description
Technical field
The invention belongs to photon crystal material field, and pH value and ionic strength response light are had concurrently more particularly, to one kind
Sub- crystal hydrogel thin film, its preparation method and application.
Background technology
Photonic crystal is a kind of periodic structure being made up of the material with different refractivity in space-alternating, its most root
This is characterized in forbidden photon band, that is, falling the light in forbidden band and being prohibited to propagate.Because its unique optical property, photon are brilliant
Body is widely used in the preparation of a variety of optics (such as modulator, sensor, display).
The photonic crystal responded with pH value and ionic strength is that mono-dispersed nano particle is dispersed in respond with pH
Optical material in property polymer.By the change of solution ph and ionic strength, Volume Changes occur for response material, so as to
Change the lattice constant of photonic crystal, Bragg diffraction peak is changed.Bore hole can intuitively observe the color occurred
Change, so as to constantly monitor the pH value of solution or ionic strength.
In anti-protein structure photon hydrogel crystal, although the ordered structure of nano-particle will not be broken by acrylic monomers
It is bad, but preparation process is cumbersome and the cycle is grown and (need to fill and go the steps such as removing template through self-assembly, monomer).It is non-tight
Although closely packed acrylamide gel can be prepared quickly, the content of its carboxyl can not be accurately controlled, limit
The repeatability of the material is made.Moreover, traditional silica and polystyrene nanoparticle its ordered structure are in extraneous bar
It is more easily damaged under part (such as temperature, solvent and mechanical force) effect, it is difficult to prepare the photon of monochromatic, large area and high quality
Crystal hydrogel thin film.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, have pH value concurrently the invention provides one kind and ionic strength is rung
Photonic crystal hydrogel thin film, its preparation method and the application answered, its object is to by using Fe3O4Nano particle and monomer
Formula, forms ordered structure in photon crystal film, thus solves existing photonic crystal hydrogel long preparation period, carboxyl
Content can not accurately control and be difficult to the photon that there is pH value and ionic strength to respond for preparing monochromatic, large area and high quality
The technical problem of crystal hydrogel thin film.
To achieve the above object, one aspect of the present invention provides a kind of photon for having pH value and ionic strength response concurrently
The preparation method of crystal hydrogel thin film, comprises the following steps：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger are dispersed in organic solvent, obtain the suspension of photonic crystal hydrogel precursor；
Contain Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 1mg~50mg, acrylamide 100mg~600mg, methyl
Hydroxy-ethyl acrylate 10mg~500mg, methylene diacrylamide 1mg~20mg, and light trigger 0.1mg~1mg；
(2) preparation of photonic crystal hydrogel thin film is solidified：By the suspension of photonic crystal hydrogel precursor in step (1)
It is paved into film；Magnetic field is loaded, above-mentioned film is developed the color, obtains the film with schemochrome；Irradiating ultraviolet light solidifies the colour developing
Film, so as to the photonic crystal hydrogel thin film solidified；Wherein, the main component of the photonic crystal hydrogel thin film of solidification
For polyacrylamide-hydroxyethyl methacrylate；
(3) preparation of photonic crystal hydrogel thin film：The photonic crystal hydrogel thin film of solidification in step (2) is immersed in
In the soluble carbonate salt aqueous solution, it is carboxyl to make the hydrolysis of ester group in polyacrylamide-hydroxyethyl methacrylate, is then soaked
In deionized water, required photonic crystal hydrogel thin film is produced；Wherein, Fe3O4The concentration of nano-particle in the film is
1mg/mL~50mg/mL.
Preferably, Fe3O4The concentration of nano-particle in the film is preferably 10mg/mL~30mg/mL, more preferably 20mg/
ML~30mg/mL.
Preferably, in step (1) organic solvent one in methanol, ethanol, ethylene glycol, polyethylene glycol, glycerine, acetone
Kind is a variety of；More preferably ethylene glycol or glycerine.
Preferably, in step (1), the Fe3O4Nano-particle is prepared as follows：By ferrocene and hydrogen peroxide
Dissolving is in acetone so that between 0.001mg/mL~0.05mg/mL, hydrogen peroxide concentration exists ferrocene concentration in the solution
Between 0.01mg/mL~0.1mg/mL；Reacted 10 hours~80 hours at 100 DEG C~500 DEG C, it is naturally cold after reaction completely
But to room temperature, solid is separated, the Fe is obtained after cleaning3O4Nano-particle.
Preferably, in step (2), the suspension in step (1) is paved into the film of 150~300 μ m-thicks, magnetic field it is strong
Spend for 300~2000 Gausses.
Preferably, in step (3), the concentration value of the soluble carbonate salt aqueous solution is 0.01g/mL~0.1g/mL；Film
Soak time in aqueous sodium carbonate is 2h；
Preferably, soluble carbonate salt is selected from sodium carbonate, potassium carbonate etc..
Another aspect provides it is a kind of have concurrently pH value and ionic strength response photonic crystal hydrogel thin film,
The film includes Fe3O4Nano-particle and polyacrylamide-metering system acid hydrogel；The Fe3O4Nano-particle is dispersed
In polyacrylamide-metering system acid hydrogel, arranged in one-dimensional chain, the concentration of nano-particle in the film is 1mg/mL
~50mg/mL.
Preferably, Fe3O4The concentration of nano-particle in the film is 10mg/mL~30mg/mL, more preferably 20mg/mL~
30mg/mL。
Preferably, the pH response spectrums scope of the film is 471nm to 673nm, and ionic strength response spectrum scope is
773nm to 552nm.
Another aspect provides the application of described photonic crystal hydrogel thin film, and it is examined applied to bore hole
Survey.
Preferably, the photonic crystal hydrogel thin film application, its described open hole detection are pH value and/or ionic strength
Double check.
Preferably, the photonic crystal hydrogel thin film is applied to biological/chemical sensor, all kinds of detectors and absorption
In indicator.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show
Beneficial effect：
(1) photonic crystal hydrogel thin film provided by the invention contains magnetic nano-particle, and its nano-particle is made in magnetic field
One dimensional arrangement can be quickly formed under, afterwards by uv photopolymerization monomer, fixes its ordered structure；Then in solubility
The hydrolysis of ester group in hydrogel is set to be carboxyl under carbonate aqueous solution effect, so as to obtain having concurrently pH value and the dual sound of ionic strength
Answer the photonic crystal hydrogel thin film of performance.
(2) preparation method of photonic crystal hydrogel provided by the invention, for nano-particle ordered structure in the external world
Under the conditions of easily destroyed problem, by by certain density Fe3O4Nano-particle and two kinds of monomers and initiator uniformly mix
Suspension is formed it into, first passing through magnetic field makes nano particle ordered arrangement, then makes its polymerization by light, is received in resulting film
Rice corpuscles ordered arrangement, shows monochrome.Meanwhile of the invention film after polymerization is immersed in the soluble carbonate salt aqueous solution makes
It is hydrolyzed, so as to be accurately controlled the content of carboxyl in hydrogel, increase repeatability, while make film in different pH value or not
Under homo-ion intensity, the visible color change of bore hole is showed, really realizes open hole detection.
(3) preparation method of the photonic crystal hydrogel thin film provided by the invention responded with pH and ionic strength,
Under the influence of externally-applied magnetic field, nano-particle quickly forms one dimensional arrangement so that preparation time is short, and whole process only needs 25 minutes left sides
The right side, and it is simple to operate, repeat by force, be easy to prepare on a large scale.
(4) by optimizing concentration value of the nano-particle in the photonic crystal hydrogel thin film containing two kinds of polymer, each
The value of material, so as to more accurately in regulation and control hydrogel carboxyl content, and obtain that preparation method is relatively easy, sensitivity is more preferable
Photonic crystal hydrogel thin film material.
(5) color of photonic crystal hydrogel thin film provided by the invention is pure, and color free from foreign meter is strong in pH value or ion
Degree has obvious color change under stimulating, and is suitable for open hole detection.
Brief description of the drawings
Fig. 1 is reflectance spectrum of the photonic crystal hydrogel thin film in different pH phosphate buffer solution in embodiment 1
Figure；
Fig. 2 be in embodiment 1 photonic crystal hydrogel thin film in the reflectance spectrum figure of the NaCl aqueous solution of various concentrations.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below that
Conflict can is not formed between this to be mutually combined.
Photonic crystal hydrogel thin film provided by the invention, including Fe3O4Nano-particle and hydrogel, the hydrogel are poly-
Acrylamide-metering system acid hydrogel；The Fe3O4Nano-particle is dispersed in polyacrylamide-methacrylic acid water-setting
In glue, the concentration of nano-particle in the film is 1mg/mL~50mg/mL, the Fe3O4Nano-particle is in one-dimensional chain under magnetic field
Shape arranges.
Photonic crystal hydrogel thin film provided by the invention, it has single color, in the cushioning liquid of different pH value
Or in the NaCl aqueous solution of various concentrations, reflecting light long displacement is big, the visible color change of bore hole is showed, is easy to bore hole to examine
Survey.The photonic crystal hydrogel thin film, can be water-soluble in soluble carbonate salt by polyacrylamide-hydroxyethyl methacrylate
The method hydrolyzed in liquid, the accurate content for controlling carboxyl in hydrogel.
Photonic crystal hydrogel thin film provided by the invention, its preparation method, comprises the following steps：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger are dispersed in organic solution, obtain the suspension of photonic crystal hydrogel precursor,
So that Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 1mg~50mg, preferably 10mg~30mg, more preferably 10mg
~20mg, preferably acrylamide 100mg~600mg, 200mg~400mg, hydroxyethyl methacrylate 10mg~500mg, preferably
20mg~40mg, more preferably 30mg~40mg, methylene diacrylamide 1mg~20mg, and light trigger 0.1mg~1mg.It is described
Light trigger be light trigger commonly used in the art, preferably 2,2- diethoxy acetophenones.The organic solvent is preferably
The conventional disperse solvent such as methanol, ethanol, ethylene glycol, polyethylene glycol, glycerine, acetone, more preferably ethylene glycol or glycerine, it is acted on
It is to more efficiently prevent from Fe3O4Nano-particle issued in magnetic field it is estranged from.
The Fe3O4Nano-particle is preferably prepared as follows：By ferrocene and hydrogen peroxide dissolving in acetone, make
In the solution ferrocene concentration between 0.001mg/mL~0.05mg/mL, hydrogen peroxide concentration 0.01mg/mL~
Between 0.1mg/mL；Reacted 10 hours~80 hours at 100 DEG C~500 DEG C, after reaction completely, naturally cool to room temperature, point
From solid, the Fe is obtained after cleaning3O4Nano-particle.
(2) preparation of photonic crystal hydrogel thin film is solidified：By the suspension of photonic crystal hydrogel precursor in step (1)
It is paved into film；Magnetic field is loaded, above-mentioned film is developed the color, obtains the film with schemochrome；Irradiating ultraviolet light solidifies the colour developing
Film, so as to the photonic crystal hydrogel thin film solidified；Wherein, the main component of the photonic crystal hydrogel thin film of solidification
For polyacrylamide-hydroxyethyl methacrylate.Wherein it is preferred in step (2), the suspension in step (1) is paved into
The film of 150 μm~300 μ m-thicks, the intensity in magnetic field are the Gauss of 300 Gausses~2000.
(3) preparation of photonic crystal hydrogel thin film：By the photonic crystal hydrogel thin film of the solidification obtained in step (2)
It is immersed in the 0.01g/mL~0.1g/mL soluble carbonate salt aqueous solution, makes in polyacrylamide-hydroxyethyl methacrylate
Hydrolysis of ester group be carboxyl；Then in immersion in deionized water, that is, the photonic crystal hydrogel thin film is made.
Wherein, soluble carbonate salt is preferably sodium carbonate or potassium carbonate.
Wherein, the time of immersion determines according to hydrolysis degree, preferably 2h.
Wherein, Fe3O4The concentration of nano-particle in the film is preferably 10mg/mL~30mg/mL, more preferably 20mg/mL
~30mg/mL.
The pH response spectrums scope of the film is 471nm to 673nm, ionic strength response spectrum scope be 773nm extremely
552nm。
The photonic crystal hydrogel thin film can be quickly prepared in the method, and whole flow process only needs 25 minutes or so, fits
Prepared for industrial-scale.
Photonic crystal hydrogel thin film provided by the invention is applied to the conventional field of various photonic crystals, such as biology/change
Learn in sensor, all kinds of detectors and adsorption indicator, in above-mentioned application, film of the invention is particularly suitable for use in bore hole inspection
Survey, especially solution ph or ionic strength open hole detection, film take on a red color, eventually become with pH reduction blueness or
Green is eventually become with the increase of ionic strength, shows the visible color change of bore hole.
It is embodiment below：
Embodiment 1
A kind of photonic crystal hydrogel thin film, is prepared as follows：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger, using ultrasonic dispersion, it is dispersed in ethylene glycol, obtains photon hydrogel crystal
The suspension of precursor so that Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 1mg, acrylamide 100mg, methyl
Hydroxy-ethyl acrylate 10mg, methylene diacrylamide 1mg, light trigger 2,2- diethoxy acetophenones 0.1mg.
The Fe3O4Nano-particle is prepared as follows：By ferrocene, hydrogen peroxide is dissolved in 75ml acetone, is obtained
Solution is added in 100mL stainless steel cauldron so that ferrocene concentration is 0.001mg/ml in the solution, and hydrogen peroxide is dense
Spend for 0.01mg/ml；Reacted 10 hours at 100 DEG C, after reaction completely, naturally cool to room temperature, separation solid obtains
Fe3O4Nano-particle, cleaned 3 times with acetone, obtain the Fe3O4Nano-particle.
(2) preparation of photonic crystal hydrogel thin film is solidified：By the photonic crystal hydrogel precursor obtained in step (1)
Suspension, between loading two glass plates, it is laid to 150 μm of film；Load the magnetic field of 300 Gausses so that the film shows
Color, obtain the film that develops the color；Irradiating ultraviolet light causes the colour developing film hardening, a length of 300nm of ultraviolet light wave.
(3) preparation of photonic crystal hydrogel thin film：The solidification photonic crystal hydrogel thin film obtained in step (2) is soaked
Bubble 2h in 0.01g/mL aqueous sodium carbonate, it is carboxylic to make the hydrolysis of ester group in polyacrylamide-hydroxyethyl methacrylate
Base；Then in immersion in deionized water, that is, the photonic crystal hydrogel thin film is made.Wherein, Fe3O4Nano-particle is thin
Concentration in film is 1mg/mL.
Embodiment 2
A kind of photonic crystal hydrogel thin film, is prepared as follows：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger, using ultrasonic dispersion, it is dispersed in glycerine, before obtaining photon hydrogel crystal
The suspension of body so that Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 1mg, acrylamide 100mg, methyl-prop
Olefin(e) acid hydroxyl ethyl ester 10mg, methylene diacrylamide 1mg, light trigger 2,2- diethoxy acetophenones 0.1mg.
The Fe3O4Nano-particle is prepared as follows：By ferrocene, hydrogen peroxide is dissolved in 75ml acetone, is obtained
Solution is added in 100mL stainless steel cauldron so that ferrocene concentration is 0.001mg/ml in the solution, and hydrogen peroxide is dense
Spend for 0.01mg/ml；Reacted 10 hours at 100 DEG C, after reaction completely, naturally cool to room temperature, separation solid obtains
Fe3O4Nano-particle, cleaned 3 times with acetone, obtain the Fe3O4Nano-particle.
(2) preparation of photonic crystal hydrogel thin film is solidified：By the photonic crystal hydrogel precursor obtained in step (1)
Suspension, between loading two glass plates, it is laid to 150 μm of film；Load the magnetic field of 300 Gausses so that the film shows
Color, obtain the film that develops the color；Irradiating ultraviolet light causes the colour developing film hardening, a length of 300nm of ultraviolet light wave.
(3) preparation of photonic crystal hydrogel thin film：The photonic crystal hydrogel thin film obtained in step (2) is immersed in
2h in 0.01g/mL aqueous sodium carbonate, it is carboxyl to make the hydrolysis of ester group in polyacrylamide-hydroxyethyl methacrylate；So
Afterwards in immersion in deionized water, that is, the photonic crystal hydrogel thin film is made.Wherein, Fe3O4Nano-particle is in the film
Concentration is 1mg/mL.
Embodiment 3
A kind of photonic crystal hydrogel thin film, is prepared as follows：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger, using ultrasonic dispersion, it is dispersed in ethylene glycol, obtains photonic crystal hydrogel
The suspension of precursor so that Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 20mg, acrylamide 200mg, first
Base hydroxy-ethyl acrylate 20mg, methylene diacrylamide 2mg, light trigger 2,2- diethoxy acetophenones 0.2mg.
The Fe3O4Nano-particle is prepared as follows：By ferrocene, hydrogen peroxide is dissolved in 75ml acetone, is obtained
Solution is added in 100mL stainless steel cauldron so that ferrocene concentration is 0.003mg/ml in the solution, and hydrogen peroxide is dense
Spend for 0.02mg/ml；Reacted 30 hours at 300 DEG C, after reaction completely, naturally cool to room temperature, separation solid obtains
Fe3O4Nano-particle, cleaned 3 times with acetone, obtain the Fe3O4Nano-particle.
(2) preparation of photonic crystal hydrogel thin film is solidified：By the photonic crystal hydrogel precursor obtained in step (1)
Suspension, between loading two glass plates, it is laid to 200 μm of film；Load the magnetic field of 500 Gausses so that the film shows
Color, obtain the film that develops the color；Irradiating ultraviolet light causes the colour developing film hardening, a length of 300nm of ultraviolet light wave.
(3) preparation of photonic crystal hydrogel thin film：The photonic crystal hydrogel thin film obtained in step (2) is immersed in
2h in 0.01g/mL aqueous sodium carbonate, it is carboxyl to make the hydrolysis of ester group in polyacrylamide-hydroxyethyl methacrylate；So
Afterwards in immersion in deionized water, that is, the photonic crystal hydrogel thin film is made.Wherein, Fe3O4Nano-particle is in the film
Concentration is 20mg/mL.
Embodiment 4
A kind of photonic crystal hydrogel thin film, is prepared as follows：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger, using ultrasonic dispersion, it is dispersed in ethylene glycol, obtains photonic crystal hydrogel
The suspension of precursor so that Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 30mg, acrylamide 400mg, first
Base hydroxy-ethyl acrylate 30mg, methylene diacrylamide 10mg, light trigger 2,2- diethoxy acetophenones 0.5mg.
The Fe3O4Nano-particle is prepared as follows：By ferrocene, hydrogen peroxide is dissolved in 75ml acetone, is obtained
Solution is added in 100mL stainless steel cauldron so that ferrocene concentration is 0.003mg/ml in the solution, and hydrogen peroxide is dense
Spend for 0.02mg/ml；Reacted 50 hours at 100 DEG C, after reaction completely, naturally cool to room temperature, separation solid obtains
Fe3O4Nano-particle, cleaned 3 times with acetone, obtain the Fe3O4Nano-particle.
(2) preparation of photonic crystal hydrogel thin film is solidified：By the photonic crystal hydrogel precursor obtained in step (1)
Suspension, between loading two glass plates, it is laid to 200 μm of film；Load the magnetic field of 300 Gausses so that the film shows
Color, obtain the film that develops the color；Irradiating ultraviolet light causes the colour developing film hardening, solidifies photon crystal film；The ultraviolet light wave
A length of 300nm.
(3) preparation of photonic crystal hydrogel thin film：The photonic crystal hydrogel thin film obtained in step (2) is immersed in
2h in 0.01g/mL aqueous sodium carbonate, it is carboxyl to make the hydrolysis of ester group in polyacrylamide-hydroxyethyl methacrylate；So
Afterwards in immersion in deionized water, that is, the photonic crystal hydrogel thin film is made.Wherein, Fe3O4Nano-particle is in the film
Concentration is 30mg/mL.
Embodiment 5
A kind of photonic crystal hydrogel thin film, is prepared as follows：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger, using ultrasonic dispersion, it is dispersed in ethylene glycol, obtains photon hydrogel crystal
The suspension of precursor so that Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 10mg, acrylamide 200mg, first
Base hydroxy-ethyl acrylate 40mg, methylene diacrylamide 2mg, light trigger 2,2- diethoxy acetophenones 0.4mg.
The Fe3O4Nano-particle is prepared as follows：By ferrocene, hydrogen peroxide is dissolved in 75ml acetone, is obtained
Solution is added in 100mL stainless steel cauldron so that ferrocene concentration is 0.002mg/ml in the solution, and hydrogen peroxide is dense
Spend for 0.03mg/ml；Reacted 50 hours at 300 DEG C, after reaction completely, naturally cool to room temperature, separation solid obtains
Fe3O4Nano-particle, cleaned 3 times with acetone, obtain the Fe3O4Nano-particle.
(2) preparation of photonic crystal hydrogel thin film is solidified：By the photonic crystal hydrogel precursor obtained in step (1)
Suspension, between loading two glass plates, it is laid to 200 μm of film；Load the magnetic field of 800 Gausses so that the film shows
Color, obtain the film that develops the color；Irradiating ultraviolet light causes the colour developing film hardening, a length of 300nm of ultraviolet light wave.
(3) preparation of photonic crystal hydrogel thin film：The photonic crystal hydrogel thin film obtained in step (2) is immersed in
2h in 0.1g/mL aqueous sodium carbonate, it is carboxyl to make the hydrolysis of ester group in polyacrylamide-hydroxyethyl methacrylate；So
Afterwards in immersion in deionized water, that is, the photonic crystal hydrogel thin film is made.Wherein, Fe3O4Nano-particle is in the film
Concentration is 10mg/mL.
Embodiment 6
A kind of photonic crystal hydrogel thin film, is prepared as follows：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger, using ultrasonic dispersion, it is dispersed in ethylene glycol, obtains photon hydrogel crystal
The suspension of precursor so that Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 10mg, acrylamide 200mg, first
Base hydroxy-ethyl acrylate 40mg, methylene diacrylamide 2mg, light trigger 2,2- diethoxy acetophenones 0.4mg.
The Fe3O4Nano-particle is prepared as follows：By ferrocene, hydrogen peroxide is dissolved in 75ml acetone, is obtained
Solution is added in 100mL stainless steel cauldron so that ferrocene concentration is 0.002mg/ml in the solution, and hydrogen peroxide is dense
Spend for 0.03mg/ml；Reacted 50 hours at 300 DEG C, after reaction completely, naturally cool to room temperature, separation solid obtains
Fe3O4Nano-particle, cleaned 3 times with acetone, obtain the Fe3O4Nano-particle.
(2) preparation of photonic crystal hydrogel thin film is solidified：By the photonic crystal hydrogel precursor obtained in step (1)
Suspension, between loading two glass plates, it is laid to 200 μm of film；Load the magnetic field of 800 Gausses so that the film shows
Color, obtain the film that develops the color；Irradiating ultraviolet light causes the colour developing film hardening, a length of 300nm of ultraviolet light wave.
(3) preparation of photonic crystal hydrogel thin film：The photonic crystal hydrogel thin film obtained in step (2) is immersed in
2h in 0.1g/mL wet chemical, it is carboxyl to make the hydrolysis of ester group in polyacrylamide-hydroxyethyl methacrylate；So
Afterwards in immersion in deionized water, that is, the photonic crystal hydrogel thin film is made.Wherein, Fe3O4Nano-particle is in the film
Concentration is 10mg/mL.
Embodiment 7
A kind of photonic crystal hydrogel thin film, is prepared as follows：
(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate,
Methylene diacrylamide and light trigger, using ultrasonic dispersion, it is dispersed in ethylene glycol, obtains photon hydrogel crystal
The suspension of precursor so that Fe in every milliliter of photonic crystal hydrogel precursor3O4Nano-particle 50mg, acrylamide 600mg, first
Base hydroxy-ethyl acrylate 500mg, methylene diacrylamide 20mg, light trigger 2,2- diethoxy acetophenones 1mg.
The Fe3O4Nano-particle is prepared as follows：By ferrocene, hydrogen peroxide is dissolved in 75ml acetone, is obtained
Solution is added in 100mL stainless steel cauldron so that ferrocene concentration is 0.05mg/ml in the solution, and hydrogen peroxide is dense
Spend for 0.1mg/ml；Reacted 80 hours at 500 DEG C, after reaction completely, naturally cool to room temperature, the Fe that separation solid obtains3O4
Nano-particle, cleaned 3 times with acetone, obtain the Fe3O4Nano-particle.
(2) preparation of photonic crystal hydrogel thin film is solidified：By the photonic crystal hydrogel precursor obtained in step (1)
Suspension, between loading two glass plates, it is laid to 300 μm of film；Load the magnetic field of 2000 Gausses so that the film shows
Color, obtain the film that develops the color；Irradiating ultraviolet light causes the colour developing film hardening, a length of 300nm of ultraviolet light wave.
(3) preparation of photonic crystal hydrogel thin film：The photonic crystal hydrogel thin film obtained in step (2) is immersed in
2h in 0.1g/mL aqueous sodium carbonate, it is carboxyl to make the hydrolysis of ester group in polyacrylamide-hydroxyethyl methacrylate；So
Afterwards in immersion in deionized water, that is, the photonic crystal hydrogel thin film is made.Wherein, Fe3O4Nano-particle is in the film
Concentration is 50mg/mL.
Embodiment 8
Photonic crystal hydrogel thin film obtained by above-described embodiment, including Fe3O4Nano-particle and polyacrylamide-first
Base acrylic hydrogel, the Fe3O4Nano-particle is dispersed in polyacrylamide-metering system acid hydrogel, described
Fe3O4Nano-particle arranges in one-dimensional chain.
By taking embodiment 1 as an example, obtained photonic crystal hydrogel thin film, including Fe3O4Nano-particle and polyacrylamide-
Metering system acid hydrogel, the Fe3O4Nano-particle is dispersed in polyacrylamide-metering system acid hydrogel, described
Fe3O4Nano-particle arranges in one-dimensional chain, the pH of photon crystal film response, i.e., when solution ph reduces from 7.03
During to 2.02, corresponding reflection spectrum peak is moved to 471nm (Fig. 1) from 673nm；The ionic strength of photonic crystal hydrogel thin film
Response：It is corresponding anti-when the concentration of NaCl in solution increases to 1.00mol/L from 0.02mol/L by taking NaCl solution as an example
Penetrate spectrum peak and be moved to 552nm (Fig. 2) from 773nm.
The photonic crystal hydrogel thin film, present it is red, eventually become with pH reduction blueness or with from
The increase of sub- intensity and eventually become green, show the visible color change of bore hole, be easy to open hole detection.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (10)
- A kind of 1. preparation method for the photonic crystal hydrogel thin film for having pH value and ionic strength response concurrently, it is characterised in that its Preparation method comprises the following steps：(1) preparation of photonic crystal hydrogel precursor：By Fe3O4Nano-particle, acrylamide, hydroxyethyl methacrylate, methene Bisacrylamide and light trigger are dispersed in organic solvent, obtain the suspension of photonic crystal hydrogel precursor；Per milli Rise in photonic crystal hydrogel precursor and contain Fe3O4Nano-particle 1mg~50mg, acrylamide 100mg~600mg, metering system Sour hydroxyl ethyl ester 10mg~500mg, methylene diacrylamide 1mg~20mg, and light trigger 0.1mg~1mg；(2) preparation of photonic crystal hydrogel thin film is solidified：The suspension of photonic crystal hydrogel precursor in step (1) is paved into Film；Magnetic field is loaded, above-mentioned film is developed the color, obtains the film with schemochrome；Irradiating ultraviolet light solidifies the colour developing film, So as to the photonic crystal hydrogel thin film solidified；Wherein, the main component of the photonic crystal hydrogel thin film of solidification is poly- Acrylamide-hydroxyethyl methacrylate；(3) preparation of photonic crystal hydrogel thin film：The photonic crystal hydrogel thin film of solidification in step (2) is immersed in solvable In the acid carbonate aqueous solution, the hydrolysis of ester group for making polyacrylamide-hydroxyethyl methacrylate is carboxyl, be then immersed in from In sub- water, required photonic crystal hydrogel thin film is produced；Wherein, Fe3O4The concentration of nano-particle in the film be 1mg/mL~ 50mg/mL。
- 2. preparation method as claimed in claim 1, it is characterised in that Fe3O4The concentration of nano-particle in the film is preferably 10mg/mL~30mg/mL.
- 3. preparation method as claimed in claim 2, it is characterised in that Fe3O4The concentration of nano-particle in the film is more preferably 20mg/mL~30mg/mL.
- 4. preparation method as claimed in claim 1, it is characterised in that in step (1), organic solvent be selected from methanol, ethanol, It is one or more in ethylene glycol, polyethylene glycol, glycerine, acetone.
- 5. preparation method as claimed in claim 1, it is characterised in that in step (2), the suspension in step (1) is spread Into the film of 150 μm~300 μ m-thicks, the intensity in magnetic field is the Gauss of 300 Gausses~2000.
- 6. preparation method as claimed in claim 1, it is characterised in that in step (3), the soluble carbonate salt aqueous solution it is dense Angle value is 0.01g/mL~0.1g/mL.
- 7. the photonic crystal hydrogel thin film that a kind of preparation method as any one of claim 1-6 is prepared, its It is characterised by：The film includes Fe3O4Nano-particle and polyacrylamide-metering system acid hydrogel；The Fe3O4Nanoparticle Son is dispersed in polyacrylamide-metering system acid hydrogel, is arranged in one-dimensional chain, Fe3O4Nano-particle is in the film Concentration be 1mg/mL~50mg/mL.
- 8. photonic crystal hydrogel thin film as claimed in claim 7, it is characterised in that the pH response spectrum scopes of the film For 471nm to 673nm, ionic strength response spectrum scope is 773nm to 552nm.
- 9. a kind of application of photonic crystal hydrogel thin film as claimed in claim 7 or 8, it is applied to open hole detection.
- 10. application as claimed in claim 9, it is characterised in that described open hole detection is the more of pH value and/or ionic strength Re-detection.
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| CN105693903B (en) * | 2016-02-02 | 2017-10-24 | 东华大学 | A kind of preparation method based on photonic crystal structure color security pattern |
| CN106040114B (en) * | 2016-05-24 | 2019-01-29 | 华中科技大学 | A kind of hydrogel photonic crystal microballoon and its preparation and application |
| CN105974611B (en) * | 2016-07-27 | 2019-01-29 | 东南大学 | The multi-functional detection contact lenses of one kind and its preparation and inspection method |
| CN107236085B (en) * | 2017-06-26 | 2019-04-16 | 北京理工大学 | A kind of method that large area quickly prepares stretching discoloration photon crystal water gel duplicature |
| CN109971005B (en) * | 2019-03-30 | 2022-02-11 | 周口师范学院 | Photonic crystal hydrogel film and preparation method and application thereof |
| CN110346330B (en) * | 2019-07-03 | 2020-11-24 | 浙江大学 | pH value detection method based on responsive thin film material |
| CN113549226B (en) * | 2020-04-24 | 2022-11-01 | 华中科技大学 | Photonic crystal hydrogel for visual bacterial detection and preparation and application thereof |
| CN112592072B (en) * | 2020-12-18 | 2022-07-19 | 武汉理工大学 | Responsive photonic crystal film with wide temperature induction interval and preparation method thereof |
| CN113736111B (en) * | 2021-08-25 | 2023-06-23 | 浙江农林大学 | Color-changing gel material, preparation method and application thereof |
| CN116854999B (en) * | 2023-09-01 | 2023-12-19 | 武汉理工大学 | Quick-response photonic crystal heterogeneous gel material, preparation method and application thereof |
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