CN102004093A - Preparation method of high-sensitiveness fluorescence detection membrane containing photonic crystal for fluorescence detection of nitric oxide - Google Patents
Preparation method of high-sensitiveness fluorescence detection membrane containing photonic crystal for fluorescence detection of nitric oxide Download PDFInfo
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- CN102004093A CN102004093A CN2010102738661A CN201010273866A CN102004093A CN 102004093 A CN102004093 A CN 102004093A CN 2010102738661 A CN2010102738661 A CN 2010102738661A CN 201010273866 A CN201010273866 A CN 201010273866A CN 102004093 A CN102004093 A CN 102004093A
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Abstract
The invention relates to a preparation method of a high-sensitiveness fluorescence detection membrane containing photonic crystal for fluorescence detection of nitric oxide. Photonic crystal is introduced into a nitric oxide fluorescence detection film, and the photonic bandgap of the photonic crystal is matched with the emission spectrum of one nitric oxide fluorescence detection molecule in the fluorescence detection film. The preparation method comprises a one-step method and a two-step method, wherein in the one-step method, nitric oxide fluorescence detection molecules are dispersed into emulsion containing monodisperse emulsion particles, and a film is formed by means of spray ink printing, spraying or spin coating; and in the two-step method, firstly, the photonic crystal film of the photonic bandgap in a visible area is obtained by means of spray ink printing, spraying, spin coating or coating, and then physical vaporous deposition or spin coating are adopted as so to disperse the nitric oxide fluorescence detection molecules for detecting nitric oxide onto the surface of the photonic crystal to obtain the high-sensitiveness fluorescence detection membrane containing photonic crystal for the fluorescence detection of nitric oxide of the photonic bandgap in the visible light area.
Description
Technical field
The invention belongs to fluorescence chemical sensor, and the applied technical field of crystal film with photon, relate in particular to the photon band gap characteristic of utilizing photonic crystal, big specific surface area and continuous duct, improve the high-sensitive preparation method who contains the fluorescent checking film of photonic crystal the nitrogen monoxide fluoroscopic examination to nitrogen monoxide fluoroscopic examination sensitivity.
Background technology
Nitrogen monoxide is prevalent in factory's discharged flue gas, mine biogas, and vehicle exhaust, various coating in the interior decoration starting material, are the important sources of air-polluting.According to statistics, the annual oxides of nitrogen of discharging in the whole world is approximately 5,300 ten thousand tons, and this wherein just comprises nitrogen monoxide.Nitrogen monoxide has very big harm to environment, and it has free radical, and character is very active; behind oxygen reaction, can generate and have corrosive gas nitrogen dioxide, serious harm human body health; cause breathing problem, even more serious illnesss such as neurasthenia.
Also have nitrogen monoxide in the biosome, the nitrogen monoxide (eNO) that human body is breathed out has reacted the health status of human body, and therefore, at biological, medical domain, nitric oxide production real-time detection is very important.People such as Gustafsson have measured the nitrogen monoxide in the breath early than 1991 and have existed.Subsequently, more bibliographical informations eNO be present in alveolar, paranasal sinus, oral cavity etc.Concerning asthma patient, the rising of eNO is its outstanding symptom.As the endothelium relaxing factor, because of Self-defense Mechanism can cause vasodilation through the nitrogen monoxide that nitricoxide synthase produces.Therefore, the measurement of nitrogen monoxide (eNO) can be used for the diagnosis of non-invasive asthma in the breath.
In recent years, along with human diagnosis, demands such as environmental quality monitoring sharply increase, and the nitric oxide production fast detecting new method of research microscratch amount has crucial meaning for timely tracking environmental quality, human body health status.Developed the fluorescence chemical sensor detection technique again in the nitric oxide production detection method of microscratch amount, the expection fluorescence chemical sensor may obtain practical application in the near future, and it comprises homogeneous fluorescent sensor, film fluorescent optical sensor and optical fiber fluorescence sensor etc.The film fluorescent optical sensor is an output signal with fluorescence, and it has highly sensitive, and good selective in addition with respect to the homogeneous fluorescent sensor, also has the advantage of not polluting system to be measured, being easy to device.Be to improve the detection sensitivity of film fluorescent optical sensor, the researchist is how strong and be beneficial to the fluorescence molecule detection film with large volume side group that is used for the film fluorescent optical sensor of nitric oxide molecule transmission with the nitric oxide molecule adhesion by design and preparation.In the existing trace amount of nitric oxide detection technique, what the past was the most frequently used is the chemiluminescence that ozone causes; Gas chromatography/mass spectrometry is analyzed and based on the spectroscopy analysis of laser.More than 3 kinds of employed instruments of method huge and expensive mostly.Commercial at present nitric oxide gas detecting device is based on electrochemical principle more, and it costs an arm and a leg, and the life-span is short, and the sensitivity of detection is low.
Develop highly sensitive, high selectivity, microscratch amount nitrogen monoxide detection technique is the problem that presses for solution at present cheaply.For further improving the sensitivity of film fluorescent optical sensor, the present invention is incorporated into photonic crystal in the nitrogen monoxide fluorescent checking film, and the photon band gap of photonic crystal and the emission spectrum of the fluorescence molecule in the fluorescent checking film are complementary, utilize the regulating and controlling effect of photonic crystal photon band gap, realize the enhancing of nitrogen monoxide fluoroscopic examination signal special wavelength light; Utilize the co-continuous cavity structure of photonic crystal, realize the nitric oxide molecule rapid diffusion of portion within it; Utilize the rough surface of photonic crystal, realize the abundant effect of its surface fluorescence molecule and nitric oxide molecule, the final enhancing that realizes nitrogen monoxide fluoroscopic examination signal increases signal to noise ratio (S/N ratio) simultaneously, improves detection sensitivity.The work of this respect yet there are no report.
Summary of the invention
The purpose of this invention is to provide a kind of with photonic crystal be incorporated into in the fluorescent checking film of nitrogen monoxide response improving nitric oxide production detection signal and to increase signal to noise ratio (S/N ratio), thereby the high-sensitive preparation method who contains the fluorescent checking film of photonic crystal to the nitrogen monoxide fluoroscopic examination is provided.
The high-sensitive preparation method who contains the fluorescent checking film of photonic crystal to the nitrogen monoxide fluoroscopic examination of the present invention comprises single stage method and two-step approach: wherein, single stage method is:
Nitrogen monoxide fluoroscopic examination molecule is distributed in the emulsion that contains single dispersed latex grain, obtains mixed liquor, the concentration of nitrogen monoxide fluoroscopic examination molecule is 10 in the mixed liquor
-4～10
-7Mol/L, the concentration of single dispersed latex grain is 0.5wt%～30wt%; Referenced patent application number: 200710179880.3 methods that proposed, under the room temperature, mixed liquor is loaded in the print cartridge that conventional ink-jet printer uses as ink-jet printing ink, base material is printed through printer by usual way then, after the printed films drying on the base material, obtain the crystal film with photon that contain nitrogen monoxide fluoroscopic examination molecule of photon band gap in the visible region, promptly obtain the large area photon band gap in the visible region (400～800nm) the high-sensitive fluorescent checking film that contains photonic crystal to the nitrogen monoxide fluoroscopic examination; Perhaps
Nitrogen monoxide fluoroscopic examination molecule and single dispersed latex grain are dispersed in the water together, obtain mixed liquor, the concentration of nitrogen monoxide fluoroscopic examination molecule is 10 in the mixed liquor
-4～10
-7Mol/L, the concentration of single dispersed latex grain is 0.5wt%～30wt%; Referenced patent application number: 200710064245.0 methods that proposed, under the room temperature, mixed liquor is loaded in the container that has conventional air gun, spray gun is aimed at selected flat substrates to spray, behind the dried coating film, obtain containing the crystal film with photon of the photon band gap of nitrogen monoxide fluoroscopic examination molecule in the visible region, promptly obtain the large area photon band gap in the visible region (400～800nm) the high-sensitive fluorescent checking film that contains photonic crystal to the nitrogen monoxide fluoroscopic examination; Perhaps
Nitrogen monoxide fluoroscopic examination molecule and single dispersed latex grain are dispersed in the water together, obtain mixed liquor, the concentration of nitrogen monoxide fluoroscopic examination molecule is 10 in the mixed liquor
-4～10
-7Mol/L, the concentration of single dispersed latex grain is 0.5wt%～30wt%; Under the room temperature, mixed liquor is spin-coated on the flat substrates, behind the dried coating film, obtain containing the crystal film with photon of the photon band gap of nitrogen monoxide fluoroscopic examination molecule in the visible region, promptly obtain the large area photon band gap in the visible region (400～800nm) the high-sensitive fluorescent checking film that contains photonic crystal to the nitrogen monoxide fluoroscopic examination.
Two-step approach comprises photon band gap preparation and two steps of the dispersion of nitrogen monoxide fluoroscopic examination molecule on the crystal film with photon of photon band gap in the visible region at the crystal film with photon of visible region:
1) photon band gap is in the preparation of the crystal film with photon of visible region:
Referenced patent application number: 200710179880.3 methods that proposed, under the room temperature, the emulsion that with concentration is single dispersed latex grain of 0.5wt%～30wt% is loaded in the print cartridge that conventional ink-jet printer uses as ink-jet printing ink, base material is printed through printer by usual way then, after the printed films drying on the base material, obtain photon band gap in the visible region (400～800nm) crystal film with photon; Perhaps
Referenced patent application number: 200710064245.0 methods that proposed, under the room temperature, with concentration is that the emulsion of single dispersed latex grain of 0.5wt%～30wt% is loaded in the container that has conventional air gun, spray gun is aimed at selected flat substrates to spray, behind the dried coating film, obtain photon band gap in the visible region (400～800nm) crystal film with photon; Perhaps
Under the room temperature, be that the emulsion of single dispersed latex grain of 0.5wt%～30wt% is spin-coated on the flat substrates with concentration, behind the dried coating film, obtain photon band gap in the visible region (400～800nm) crystal film with photon; Perhaps
Referenced patent application number: the method that CN:200510011219.2 proposed, under the room temperature, earlier single dispersed latex grain is dispersed in the water, obtain containing the emulsion of single dispersed latex grain, the concentration of the single dispersed latex grain in the emulsion is 0.5wt%～30wt%; The emulsion that will contain single dispersed latex grain then evenly covers on the flat substrates, treat just to obtain after the aqueous solvent volatilization photon band gap in the visible region (400～800nm) crystal film with photon;
2) dispersion of nitrogen monoxide fluoroscopic examination molecule on the crystal film with photon of photon band gap in the visible region
Can pass through physical vaporous deposition, the photon band gap that solid nitrogen monoxide fluoroscopic examination molecule evaporation is obtained to step 1) is on the crystal film with photon surface of visible region, (400～800nm) crystal film with photon surface forms one deck nitrogen monoxide fluoroscopic examination molecular film, obtains the high-sensitive fluorescent checking film that contain photonic crystal to nitrogen monoxide fluoroscopic examination of large area photon band gap in the visible region in the visible region at photon band gap; Wherein, the thickness of nitrogen monoxide fluoroscopic examination molecular film is 10nm～80nm; Or
By spin-coating method, nitrogen monoxide fluoroscopic examination molecular solution is spun to photon band gap that step 1) obtains on the crystal film with photon surface of visible region, the concentration of nitrogen monoxide fluoroscopic examination molecule is 10 in the solution
-4～10
-7Mol/L, form one deck nitrogen monoxide fluoroscopic examination molecular film at photon band gap on the crystal film with photon surface of visible region, obtain the large area photon band gap in the visible region (400～800nm) the high-sensitive fluorescent checking film that contains photonic crystal to the nitrogen monoxide fluoroscopic examination, wherein, the thickness of nitrogen monoxide fluoroscopic examination molecular film is 10nm～80nm.
The high-sensitive fluorescent checking film that contains photonic crystal to the nitrogen monoxide fluoroscopic examination of the present invention, the sensitivity of the existing fluorescent checking film that does not contain photonic crystal when nitrogen monoxide is detected of comparison nitrogen monoxide fluoroscopic examination can improve 50 times.
Described base material comprises: paper, glass, silicon chip or metal (comprising aluminium or copper etc.) film etc.
Described nitrogen monoxide fluoroscopic examination molecular solution obtains nitrogen monoxide fluoroscopic examination molecular melting in organic solvent, wherein, described organic solvent is absolute ethyl alcohol, chloroform, dimethyl sulfoxide (DMSO) (DMSO) or N, dinethylformamide (DMF) etc.
Described nitrogen monoxide fluoroscopic examination molecule is a diamido fluorescein (DAF-2) etc.
Photon band gap among the present invention is piled up by single dispersed latex grain at the crystal film with photon of visible region and is formed, the crystal film with photon of photon band gap in the visible region has the duct (duct that the slit between single dispersed latex grain forms) of micron and/or sub-micron, and the particle size range of single dispersed latex grain is preferably 170～300nm.
Single dispersed latex grain among the present invention comprises single organic high molecular emulsion grain or single inorganic oxide emulsion particle that disperses of disperseing.
The organic high molecular emulsion grain of described single dispersion is single triblock polymer emulsion particle, monodisperse polystyrene emulsion particle or single polymethylmethacrylate emulsion particle that disperses of disperseing of hard core-soft core structure.Described single dispersion inorganic oxide emulsion particle is monodisperse silica emulsion particle or monodisperse titanium dioxide emulsion particle.
The described emulsion that contains single dispersed latex grain obtains after at room temperature being dispersed in single dispersed latex grain in the water, as the concentration that obtains the single dispersed latex grain in the emulsion is 0.5wt%～30wt%; Also can use for reference the method that patent ZL200510011219.2 is proposed, take the batch method emulsifier-free emulsion polymerization, by adjusting emulsion polymerization technique, can single stage method prepare the single emulsion of disperseing the triblock polymer emulsion particle that contains hard core-soft core structure, the particle diameter preferable range of single dispersion triblock polymer emulsion particle of the hard core-soft core structure that it prepares is 170～300nm.
Described single triblock polymer emulsion particle that disperses is poly-(styrene-methyl methacrylate-acrylic acid) emulsion particle, poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle, poly-(styrene-methyl methacrylate-acrylamide) emulsion particle or poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle.
Design of the present invention is that photonic crystal is incorporated in the nitrogen monoxide fluorescent checking film, and the emission spectrum to the nitrogen monoxide fluoroscopic examination molecule of nitrogen monoxide response in the photon band gap of photonic crystal and the fluorescent checking film is complementary.The preparation method comprises single stage method and two-step approach.Single stage method is that nitrogen monoxide fluoroscopic examination molecule is distributed in the emulsion that contains single dispersed latex grain, by inkjet printing, spraying or spin coating mode film forming; Two-step approach at first obtains the crystal film with photon of photon band gap in the visible region by inkjet printing, spraying, spin coating or coating method; Adopt physical vaporous deposition then or adopt spin-coating method, to detect nitric oxide production nitrogen monoxide fluoroscopic examination molecule and be distributed to the crystal film with photon surface, obtain the high-sensitive fluorescent checking film that contain photonic crystal to nitrogen monoxide fluoroscopic examination of photon band gap in the visible region.And the emission spectrum of the photon band gap of photonic crystal and nitrogen monoxide fluoroscopic examination molecule is complementary, and utilizes the regulating and controlling effect of photonic crystal to special wavelength light, realizes the enhancing of fluoroscopic examination signal; The air duct that the structure of utilizing photonic crystal to have co-continuous forms is realized the nitric oxide molecule rapid diffusion of portion within it; Utilize the rough surface of photonic crystal, realize the abundant effect of its surperficial nitrogen monoxide fluoroscopic examination molecule and nitric oxide molecule, realize the enhancing of detection signal, with final raising detection sensitivity.
The invention will be further described below in conjunction with accompanying drawing and by embodiment.
Description of drawings
The sem photograph to the fluorescent checking film that contain photonic crystal of nitrogen monoxide fluoroscopic examination of Fig. 1 for obtaining in the embodiment of the invention 1.
Fig. 2 (a) detects the nitrogen monoxide synoptic diagram for the fluorescent checking film that does not contain photonic crystal to the nitrogen monoxide fluoroscopic examination that obtains in the embodiment of the invention 1.
Fig. 2 (b) detects the nitrogen monoxide synoptic diagram for the fluorescent checking film that contains photonic crystal to the nitrogen monoxide fluoroscopic examination that obtains in the embodiment of the invention 1.
Fig. 3 is in the embodiment of the invention 1, and the fluorescent checking film that does not contain photonic crystal of nitrogen monoxide fluoroscopic examination is detected nitric oxide production fluorescence spectrum figure.0: blank glass surface fluorescence spectrogram; 1: the spin coating fluorescence molecule detects the fluorescence spectrum figure of the detection film that makes behind the solution; 2: detect film and detect nitrogen monoxide fluorescence spectrum figure.
Fig. 4 is in the embodiment of the invention 1, and the fluorescent checking film that contains photonic crystal of nitrogen monoxide fluoroscopic examination is detected nitric oxide production fluorescence spectrum figure.0: the brilliant surface fluorescence spectrogram of blank light; 1: the spin coating fluorescence molecule detects the fluorescence spectrum figure of the detection film that makes behind the solution; 2: the brilliant film that detects of light detects nitrogen monoxide fluorescence spectrum figure.
Fig. 5 is in the embodiment of the invention 1, detects nitric oxide production fluorescence spectrum figure to the fluorescent checking film that contains photonic crystal of nitrogen monoxide fluoroscopic examination with to the fluorescent checking film that does not contain photonic crystal of nitrogen monoxide fluoroscopic examination: 0 and 1 respectively to the fluorescence spectrum of the fluorescent checking film that does not contain photonic crystal of nitrogen monoxide fluoroscopic examination with to the fluorescence spectrum of the fluorescent checking film that contains photonic crystal of nitrogen monoxide fluoroscopic examination.Can obviously find out by figure, because the introducing of photonic crystal makes fluorescence intensity increase about 50 times.
Embodiment
Nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is distributed to contain particle diameter be that the single of 243nm disperses in poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle solution, obtain mixed liquor, the concentration of fluorescence molecule diamido fluorescein is 10 in the mixed liquor
-7Mol/L, the concentration of poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle of single dispersion is 20wt%; Under the room temperature (25 ℃), mixed liquor is spin-coated on glass, behind the dried coating film, obtain containing the crystal film with photon of the photon band gap of nitrogen monoxide fluoroscopic examination molecule diamido fluorescein in 400～800nm visible region, promptly obtain the high-sensitive fluorescent checking film that contain photonic crystal to nitrogen monoxide fluoroscopic examination of large area photon band gap in the visible region, sem photograph as shown in Figure 1; Photon band gap disperses poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle to pile up and form at the crystal film with photon of visible region by single, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.Detect nitric oxide production synoptic diagram shown in Fig. 2 (b) with this detection film to the nitrogen monoxide fluoroscopic examination; Fluorescence spectrum figure as shown in Figure 4, wherein: 0: the brilliant surface fluorescence spectrogram of blank light; 1: the spin coating fluorescence molecule detects the fluorescence spectrum figure of the detection film that makes behind the solution; 2: the brilliant film that detects of light detects nitrogen monoxide fluorescence spectrum figure.
As a comparison, nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is soluble in water, and the concentration of diamido fluorescein is 10 in the gained solution
-7Mol/L is spun to glass surface with gained solution, prepares detection film to the nitrogen monoxide fluoroscopic examination at glass surface, does not promptly contain the detection film to the nitrogen monoxide fluoroscopic examination of photonic crystal, and it can detect nitrogen monoxide.Detect nitric oxide production synoptic diagram shown in Fig. 2 (a) with this detection film to the nitrogen monoxide fluoroscopic examination; Fluorescence spectrum figure as shown in Figure 3, wherein: 0: blank glass surface fluorescence spectrogram; 1: the spin coating fluorescence molecule detects the fluorescence spectrum figure of the detection film that makes behind the solution; 2: detect film and detect nitrogen monoxide fluorescence spectrum figure.
Fluorescence spectrum as shown in Figure 5, under the same conditions, detect nitrogen monoxide respectively, from fluorescence spectrum figure, can obviously find out with the fluorescent checking film that contains the nitrogen monoxide fluorescent checking film of photonic crystal and do not contain photonic crystal, because the introducing of photonic crystal makes fluorescence intensity increase about 50 times.Among the figure 0 and 1 is respectively to the fluorescence spectrum of the fluorescent checking film that does not contain photonic crystal of nitrogen monoxide fluoroscopic examination with to the fluorescence spectrum of the fluorescent checking film that contains photonic crystal of nitrogen monoxide fluoroscopic examination.
Be that 243nm single disperse poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle to be dispersed in to obtain single dispersed latex grain concentration in the water with particle diameter be the solution of 0.5wt%, under the room temperature (25 ℃), mixed liquor is spin-coated on glass, obtains the crystal film with photon of photon band gap after the drying in 400～800nm visible region.With nitrogen monoxide fluoroscopic examination molecule diamido fluorescein with 10
-7Concentration is soluble in water, and (on preparation-obtained crystal film with photon, wherein, the thickness of fluorescence molecule deposited film is 80nm in spin coating.Resultant large area photon band gap is at the high-sensitive fluorescent checking film that contains photonic crystal to the nitrogen monoxide fluoroscopic examination of visible region.Photon band gap disperses poly-(styrene-methyl methacrylate-acrylic acid) emulsion particle to pile up and form at the crystal film with photon of visible region by single, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.
Embodiment 3.
With reference to the method that CN:200710179880.3 proposed, under room temperature (25 ℃), with particle diameter is that the monodisperse titanium dioxide emulsion particle of 243nm is dispersed in the water, obtain containing the emulsion of single dispersed latex grain, the concentration of the single dispersed latex grain in the emulsion is 20wt%, then resulting single dispersed latex grain emulsion is loaded in the print cartridge that conventional ink-jet printer uses as ink-jet printing ink, glass baseplate is printed through printer by usual way then, after the printed films drying, obtain the crystal film with photon of large area photon band gap at glass surface in 400～800nm visible region, photon band gap is piled up by the monodisperse titanium dioxide emulsion particle at the crystal film with photon of visible region and is formed, and has the duct of micron and/or sub-micron.Nitrogen monoxide fluoroscopic examination molecule diamido fluorescein (DAF-2) is dissolved in the chloroform, and the concentration of nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is 10 in the gained solution
-5Mol/L is spun to gained solution above-mentioned crystal film with photon surface (thickness of the diamido fluorescein film that deposition forms is 10nm) then, obtains the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region.
Embodiment 4.
Under room temperature (25 ℃), nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is distributed to contain particle diameter be that 243nm single disperses in the emulsion of poly-(styrene-methyl methacrylate-acrylic acid) emulsion particle, obtain mixed liquor, the concentration of fluorescence molecule diamido fluorescein is 10 in the mixed liquor
-4Mol/L, the concentration of poly-(styrene-methyl methacrylate-acrylic acid) emulsion particle of single dispersion is 30wt%; With reference to the method that CN:200710179880.3 proposed, under the room temperature, mixed liquor is loaded in the print cartridge that conventional ink-jet printer uses as ink-jet printing ink, paper substrate is printed through printer by usual way then, after the printed films drying, obtain containing the crystal film with photon of the photon band gap of nitrogen monoxide fluoroscopic examination molecule diamido fluorescein on the paper surface, promptly obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of large area photon band gap in the visible region in 400～800nm visible region; Photon band gap disperses poly-(styrene-methyl methacrylate-acrylic acid) emulsion particle to pile up and form at the crystal film with photon of visible region by single, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Embodiment 5.
Under room temperature (25 ℃), be that single dispersed latex grain polystyrene of 230nm is dispersed in the water together with nitrogen monoxide fluoroscopic examination molecule diamido fluorescein and particle diameter, obtain mixed liquor, the concentration of fluorescence molecule diamido fluorescein is 10 in the mixed liquor
-4Mol/L, the concentration of single dispersed latex grain polystyrene is 15wt%, with reference to the method that CN:200710064245.0 proposed, under the room temperature, mixed liquor is loaded in the container that has conventional air gun, spray gun is aimed at selected glass to spray, behind the dried coating film, obtain containing the crystal film with photon of the photon band gap of nitrogen monoxide fluoroscopic examination molecule diamido fluorescein, promptly obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of large area photon band gap in the visible region in 400～800nm visible region; Photon band gap is piled up by single dispersed latex grain polystyrene at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Embodiment 6.
Under room temperature (25 ℃), with reference to the method that CN:200510011219.2 proposed, the monodisperse titanium dioxide emulsion particle that with particle diameter is 230nm earlier is dispersed in the water, obtain containing the emulsion of monodisperse titanium dioxide emulsion particle, the concentration of the single dispersed latex grain in the emulsion is 0.5wt%, evenly cover the resulting emulsion that contains the monodisperse titanium dioxide emulsion particle on the copper sheet then, treat just to obtain the crystal film with photon of photon band gap after the aqueous solvent volatilization in 400～800nm visible region, adopt physical vaporous deposition then, with solid nitrogen monoxide fluoroscopic examination molecule diamido fluorescein evaporation to the crystal film with photon surface, form one deck nitrogen monoxide fluoroscopic examination molecule diamido fluorescein film on the crystal film with photon surface of 400～800nm visible region at photon band gap, obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region, wherein, the thickness of nitrogen monoxide fluorescence molecule deposited film is 80nm, photon band gap is piled up by the monodisperse titanium dioxide emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Embodiment 7.
Under room temperature (25 ℃), with reference to the method that CN:200510011219.2 proposed, be earlier that the single of 230nm disperses poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle to be dispersed in the water with particle diameter, obtain containing single emulsion of disperseing poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle, the concentration of poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle of single dispersion in the emulsion is 10wt%, then resulting single emulsion of poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle of disperseing evenly is spin-coated on the silicon chip, treats just to obtain the crystal film with photon of photon band gap after the aqueous solvent volatilization in 400～800nm visible region.Nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is dissolved among the DMF, and the concentration of nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is 10 in the gained solution
-4Mol/L, then gained solution is spun to above-mentioned crystal film with photon surface, form one deck nitrogen monoxide fluoroscopic examination molecule diamido fluorescein film on the crystal film with photon surface of 400～800nm visible region at photon band gap, obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region, wherein, the thickness of the diamido fluorescein film that deposition forms is 80nm, photon band gap is piled up by the monodisperse titanium dioxide emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Embodiment 8.
With reference to the method that CN:200710064245.0 proposed, under room temperature (25 ℃), with particle diameter is that the monodisperse silica emulsion particle of 230nm is dispersed in the water, obtain containing the emulsion of monodisperse silica emulsion particle, the concentration of the monodisperse silica emulsion particle in the emulsion is 15wt%, emulsion with resulting monodisperse silica emulsion particle is loaded in the container that has conventional air gun then, spray gun is aimed at selected glass to spray, behind the dried coating film, obtain the crystal film with photon of photon band gap in 400～800nm visible region.Adopt physical vaporous deposition then, solid nitrogen monoxide fluoroscopic examination molecule diamido fluorescein evaporation is arrived above-mentioned crystal film with photon surface, form one deck nitrogen monoxide fluoroscopic examination molecule diamido fluorescein film on the crystal film with photon surface of 400～800nm visible region at photon band gap, obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region, wherein, the thickness of the diamido fluorescein film that deposition forms is 40nm, photon band gap is piled up by the monodisperse silica emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has micron and/or the duct of sub-micron, and it can detect nitrogen monoxide.
Embodiment 9.
With reference to the method that CN:200710064245.0 proposed, under room temperature (25 ℃), with particle diameter is that the single of 179nm disperses poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle to be dispersed in the water, obtain containing single emulsion of disperseing poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle, the concentration of poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle of single dispersion in the emulsion is 25wt%, then the resulting emulsion that contains poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle of single dispersion is loaded in the container that has conventional air gun, spray gun is aimed at selected glass to spray, behind the dried coating film, obtain the crystal film with photon of photon band gap in 400～800nm visible region.Nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is dissolved in the dimethyl sulfoxide (DMSO) (DMSO), and the concentration of nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is 10 in the gained solution
-7Mol/L, then gained solution is spun to above-mentioned crystal film with photon surface, form one deck nitrogen monoxide fluoroscopic examination molecule diamido fluorescein film on the crystal film with photon surface of 400～800nm visible region at photon band gap, obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region, wherein, the thickness of the diamido fluorescein film that deposition forms is 30nm, photon band gap is piled up by the monodisperse silica emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Embodiment 10.
With reference to the method that CN:200710179880.3 proposed, under room temperature (25 ℃), with particle diameter is that the monodisperse titanium dioxide emulsion particle of 230nm is dispersed in the water, obtain containing the emulsion of monodisperse titanium dioxide emulsion particle, the concentration of the monodisperse titanium dioxide emulsion particle in the emulsion is 30wt%, then the resulting emulsion that contains single dispersed latex grain is loaded in the print cartridge that conventional ink-jet printer uses as ink-jet printing ink, paper substrate is printed through printer by usual way then, after the printed films drying, obtain the crystal film with photon of large area photon band gap on the paper surface in 400～800nm visible region.Adopt physical vaporous deposition then, solid nitrogen monoxide fluoroscopic examination molecule diamido fluorescein evaporation is arrived above-mentioned crystal film with photon surface, form one deck nitrogen monoxide fluoroscopic examination molecule diamido fluorescein film on the crystal film with photon surface of 400～800nm visible region at photon band gap, obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region, wherein, the thickness of the diamido fluorescein film that deposition forms is 20nm, photon band gap is piled up by the monodisperse titanium dioxide emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Embodiment 11.
With reference to the method that CN:200710179880.3 proposed, under room temperature (25 ℃), with particle diameter is that single polymethylmethacrylate emulsion particle that disperses of 179nm is dispersed in the water, obtain containing single emulsion of disperseing poly-polymethylmethacrylate emulsion particle, the concentration of the single dispersion polymethylmethacrylate emulsion particle in the emulsion is 15wt%, contain single emulsion of disperseing the polymethylmethacrylate emulsion particle and be loaded in the print cartridge that conventional ink-jet printer uses resulting then as ink-jet printing ink, paper substrate is printed through printer by usual way then, after the printed films drying, obtain the crystal film with photon of large area photon band gap on the paper surface in 400～800nm visible region.Nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is dissolved among the DMF, and the concentration of fluorescence molecule diamido fluorescein is 10 in the gained solution
-5Mol/L, then gained solution is spun to above-mentioned crystal film with photon surface, form one deck nitrogen monoxide fluoroscopic examination molecule diamido fluorescein film on the crystal film with photon surface of 400～800nm visible region at photon band gap, obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region, wherein, the thickness of the diamido fluorescein film that deposition forms is 10nm, photon band gap is piled up by the monodisperse titanium dioxide emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Embodiment 12.
Under room temperature (25 ℃), the monodisperse titanium dioxide emulsion particle that will contain particle diameter and be 230nm is dispersed in the water, obtain containing the emulsion of monodisperse titanium dioxide emulsion particle, the concentration of the monodisperse titanium dioxide emulsion particle in the emulsion is 20wt%, be spin-coated on the resulting emulsion that contains the monodisperse titanium dioxide emulsion particle on glass then, behind the dried coating film, obtain the crystal film with photon of photon band gap in 400～800nm visible region.Adopt physical vaporous deposition then, solid nitrogen monoxide fluoroscopic examination molecule diamido fluorescein evaporation is arrived above-mentioned crystal film with photon surface, form one deck nitrogen monoxide fluoroscopic examination molecule diamido fluorescein film on the crystal film with photon surface of 400～800nm visible region at photon band gap, obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region, wherein, the thickness of the diamido fluorescein film that deposition forms is 40nm, photon band gap is piled up by the monodisperse titanium dioxide emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Embodiment 13.
Under room temperature (25 ℃), the monodisperse titanium dioxide emulsion particle that will contain particle diameter and be 179nm is dispersed in the water, obtain containing the emulsion of monodisperse titanium dioxide emulsion particle, the concentration of the monodisperse titanium dioxide emulsion particle in the emulsion is 15wt%, then the resulting emulsion that contains the monodisperse titanium dioxide emulsion particle is spin-coated on the aluminium flake, behind the dried coating film, obtain the crystal film with photon of photon band gap in 400～800nm visible region.Nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is dissolved in the absolute ethyl alcohol, and the concentration of nitrogen monoxide fluoroscopic examination molecule diamido fluorescein is 10 in the gained solution
-6Mol/L, then gained solution is spun to above-mentioned crystal film with photon surface, form one deck nitrogen monoxide fluoroscopic examination molecule diamido fluorescein film on the crystal film with photon surface of 400～800nm visible region at photon band gap, obtain the high-sensitive nitrogen monoxide fluorescent checking film that contain photonic crystal of photon band gap in the visible region, wherein, the thickness of the diamido fluorescein film that deposition forms is 20nm, photon band gap is piled up by the monodisperse titanium dioxide emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.It can detect nitrogen monoxide.
Claims (10)
1. high-sensitive preparation method who contains the fluorescent checking film of photonic crystal to the nitrogen monoxide fluoroscopic examination is characterized in that:
Nitrogen monoxide fluoroscopic examination molecule is distributed in the emulsion that contains single dispersed latex grain, obtains mixed liquor, the concentration of nitrogen monoxide fluoroscopic examination molecule is 10 in the mixed liquor
-4～10
-7Mol/L, the concentration of single dispersed latex grain is 0.5wt%～30wt%; Under the room temperature, mixed liquor is loaded in the print cartridge that conventional ink-jet printer uses as ink-jet printing ink, base material is printed through printer by usual way then, after the printed films drying on the base material, obtain the crystal film with photon that contain nitrogen monoxide fluoroscopic examination molecule of photon band gap, promptly obtain the high-sensitive fluorescent checking film that contain photonic crystal to nitrogen monoxide fluoroscopic examination of photon band gap in the visible region in the visible region; Perhaps
Nitrogen monoxide fluoroscopic examination molecule and single dispersed latex grain are dispersed in the water together, obtain mixed liquor, the concentration of nitrogen monoxide fluoroscopic examination molecule is 10 in the mixed liquor
-4～10
-7Mol/L, the concentration of single dispersed latex grain is 0.5wt%～30wt%; Under the room temperature, mixed liquor is loaded in the container that has conventional air gun, spray gun is aimed at selected flat substrates to spray, behind the dried coating film, obtain the crystal film with photon that contain nitrogen monoxide fluoroscopic examination molecule of photon band gap, promptly obtain the high-sensitive fluorescent checking film that contain photonic crystal to nitrogen monoxide fluoroscopic examination of photon band gap in the visible region in the visible region; Perhaps
Nitrogen monoxide fluoroscopic examination molecule and single dispersed latex grain are dispersed in the water together, obtain mixed liquor, the concentration of nitrogen monoxide fluoroscopic examination molecule is 10 in the mixed liquor
-4～10
-7Mol/L, the concentration of single dispersed latex grain is 0.5wt%～30wt%; Under the room temperature, mixed liquor is spin-coated on the flat substrates, behind the dried coating film, obtain the crystal film with photon that contain nitrogen monoxide fluoroscopic examination molecule of photon band gap, promptly obtain the high-sensitive fluorescent checking film that contain photonic crystal to nitrogen monoxide fluoroscopic examination of photon band gap in the visible region in the visible region;
Described single dispersed latex grain comprises single organic high molecular emulsion grain or single inorganic oxide emulsion particle that disperses of disperseing.
2. high-sensitive preparation method who contains the fluorescent checking film of photonic crystal to the nitrogen monoxide fluoroscopic examination is characterized in that:
1) under the room temperature, the emulsion that with concentration is single dispersed latex grain of 0.5wt%～30wt% is loaded in the print cartridge that conventional ink-jet printer uses as ink-jet printing ink, base material is printed through printer by usual way then, after the printed films drying on the base material, obtain the crystal film with photon of photon band gap in the visible region; Perhaps
Under the room temperature, with concentration is that the emulsion of single dispersed latex grain of 0.5wt%～30wt% is loaded in the container that has conventional air gun, spray gun is aimed at selected flat substrates spray, behind the dried coating film, obtain the crystal film with photon of photon band gap in the visible region; Perhaps
Under the room temperature, be that the emulsion of single dispersed latex grain of 0.5wt%～30wt% is spin-coated on the flat substrates, behind the dried coating film, obtain the crystal film with photon of photon band gap in the visible region with concentration; Perhaps
Under the room temperature, earlier single dispersed latex grain is dispersed in the water, obtains containing the emulsion of single dispersed latex grain, the concentration of the single dispersed latex grain in the emulsion is 0.5wt%～30wt%; The emulsion that will contain single dispersed latex grain then evenly covers on the flat substrates, treats just to obtain the crystal film with photon of photon band gap in the visible region after the aqueous solvent volatilization;
2) pass through physical vaporous deposition, the photon band gap that solid nitrogen monoxide fluoroscopic examination molecule evaporation is obtained to step 1) is on the crystal film with photon surface of visible region, form one deck nitrogen monoxide fluoroscopic examination molecular film at photon band gap on the crystal film with photon surface of visible region, obtain the high-sensitive fluorescent checking film that contain photonic crystal to nitrogen monoxide fluoroscopic examination of photon band gap in the visible region; Or
By spin-coating method, nitrogen monoxide fluoroscopic examination molecular solution is spun to photon band gap that step 1) obtains on the crystal film with photon surface of visible region, the concentration of nitrogen monoxide fluoroscopic examination molecule is 10 in the solution
-4～10
-7Mol/L forms one deck nitrogen monoxide fluoroscopic examination molecular film at photon band gap on the crystal film with photon surface of visible region, obtains the high-sensitive fluorescent checking film that contain photonic crystal to nitrogen monoxide fluoroscopic examination of photon band gap in the visible region;
Described single dispersed latex grain comprises single organic high molecular emulsion grain or single inorganic oxide emulsion particle that disperses of disperseing.
3. method according to claim 1 and 2, it is characterized in that: the described high-sensitive fluorescent checking film that contains photonic crystal to the nitrogen monoxide fluoroscopic examination, the sensitivity of the fluorescent checking film that does not contain photonic crystal when nitrogen monoxide is detected of comparison nitrogen monoxide fluoroscopic examination improves 50 times.
4. method according to claim 1 and 2 is characterized in that: described nitrogen monoxide fluoroscopic examination molecule is the diamido fluorescein.
5. method according to claim 2 is characterized in that: the thickness of described nitrogen monoxide fluoroscopic examination molecular film is 10nm～80nm.
6. method according to claim 1 and 2; it is characterized in that: described photon band gap is piled up by single organic high molecular emulsion grain of dispersion or single dispersion inorganic oxide emulsion particle at the crystal film with photon of visible region and is formed, and the crystal film with photon of photon band gap in the visible region has the duct of micron and/or sub-micron.
7. method according to claim 1 and 2 is characterized in that: the organic high molecular emulsion grain of described single dispersion is single triblock polymer emulsion particle, monodisperse polystyrene emulsion particle or single polymethylmethacrylate emulsion particle that disperses of disperseing of hard core-soft core structure; Described single dispersion inorganic oxide emulsion particle is monodisperse silica emulsion particle or monodisperse titanium dioxide emulsion particle.
8. method according to claim 6 is characterized in that: the organic high molecular emulsion grain of described single dispersion is single triblock polymer emulsion particle, monodisperse polystyrene emulsion particle or single polymethylmethacrylate emulsion particle that disperses of disperseing of hard core-soft core structure; Described single dispersion inorganic oxide emulsion particle is monodisperse silica emulsion particle or monodisperse titanium dioxide emulsion particle.
9. method according to claim 7 is characterized in that: described single triblock polymer emulsion particle that disperses is poly-(styrene-methyl methacrylate-acrylic acid) emulsion particle, poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle, poly-(styrene-methyl methacrylate-acrylamide) emulsion particle or poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle.
10. method according to claim 8 is characterized in that: described single triblock polymer emulsion particle that disperses is poly-(styrene-methyl methacrylate-acrylic acid) emulsion particle, poly-(methyl styrene-methyl methacrylate-acrylic acid) emulsion particle, poly-(styrene-methyl methacrylate-acrylamide) emulsion particle or poly-(methyl styrene-methyl methacrylate-acrylamide) emulsion particle.
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