CN115575372A - Method for manufacturing oxygen sensor fluorescent film, oxygen sensor fluorescent film and oxygen sensor - Google Patents
Method for manufacturing oxygen sensor fluorescent film, oxygen sensor fluorescent film and oxygen sensor Download PDFInfo
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- CN115575372A CN115575372A CN202211330204.2A CN202211330204A CN115575372A CN 115575372 A CN115575372 A CN 115575372A CN 202211330204 A CN202211330204 A CN 202211330204A CN 115575372 A CN115575372 A CN 115575372A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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Abstract
The method for manufacturing the oxygen sensor fluorescent film, the oxygen sensor fluorescent film and the oxygen sensor comprises the following steps: s1: coating a fluorescence indicator in a ZIF-8 material to obtain a ZIF-8 composite material coated with the fluorescence indicator; s2: preparing a fluorescent layer mixed solution, wherein the fluorescent layer mixed solution contains a ZIF-8 composite material coated with a fluorescent indicator; s3: providing a substrate, and solidifying the fluorescent layer mixed solution on the substrate to form a fluorescent layer on the substrate; s4: and forming a shading breathable layer on one side of the fluorescent layer, which is far away from the substrate. The oxygen sensor manufactured by the method can improve the dispersion degree and the uniformity of the fluorescent indicator on the carrier, improve the air permeability of the fluorescent film of the oxygen sensor, improve the sensitivity of the oxygen sensor to oxygen and shorten the response time.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a manufacturing method of an oxygen sensor fluorescent film, the oxygen sensor fluorescent film and an oxygen sensor.
Background
The determination of gaseous oxygen or dissolved oxygen concentration is required in many fields such as biology, medicine, environment, industrial processes, etc.
Compared with the traditional oxygen sensing technology, the fluorescence-oxygen sensing technology based on the fluorescence quenching effect has the characteristics of high response speed, short balance time, no oxygen consumption in the test process, low-temperature working and the like. Because of the above advantages, the fluorescent oxygen sensor has been widely used internationally in the fields of chemistry, biology, clinical medicine, environmental monitoring, and the like.
The fluorescence quenching effect is mainly that oxygen is used for quenching the fluorescence of some fluorescent substances, and the oxygen content is judged according to the fluorescence intensity or quenching time. A key component of a fluorescence-oxygen sensor is the fluorescent oxygen-sensitive membrane material that can produce fluorescent emissions. The sensitive membrane is generally formed by embedding a fluorescent compound in a solid matrix and then coating the solid matrix to form a membrane.
The development of technology places increasing demands on the response speed of fluorescence-oxygen sensors. Based on the principle and the structure, the loading capacity and the dispersion degree of fluorescent indicator molecules on a carrier and the oxygen permeability of a film-forming organic matrix are the key points for restricting the improvement of the response speed of the fluorescence-oxygen sensor.
Disclosure of Invention
In view of the above, the present invention provides a method for manufacturing an oxygen sensor fluorescent film, an oxygen sensor fluorescent film and an oxygen sensor, the method can improve the dispersion degree and uniformity of a fluorescent indicator on a carrier, improve the air permeability of the oxygen sensor fluorescent film, improve the sensitivity of the oxygen sensor to oxygen, and shorten the response time.
The invention provides a method for manufacturing an oxygen sensor fluorescent film, which comprises the following steps:
s1: coating a fluorescent indicator in a ZIF-8 material to obtain a ZIF-8 composite material coated with the fluorescent indicator;
s2: preparing a fluorescent layer mixed solution, wherein the fluorescent layer mixed solution contains a ZIF-8 composite material coated with a fluorescent indicator;
s3: providing a substrate, and solidifying the fluorescent layer mixed solution on the substrate to form a fluorescent layer on the substrate;
s4: and forming a light-shading breathable layer on one side of the fluorescent layer, which is far away from the substrate.
Further, in forming the fluorescent indicator coated ZIF-8 composite, the method further comprises:
dissolving zinc nitrate hexahydrate in the solution A, and adding a surfactant to obtain a solution A containing zinc ions; dissolving 2-methylimidazole and a fluorescent indicator in the solution B to obtain a solution B containing the fluorescent indicator and 2-methylimidazole;
and mixing the solution A and the solution B, and stirring, centrifuging and drying to obtain the ZIF-8 composite material coated with the fluorescent indicator.
Further, the solution A is a methanol solution, and the solution B is a mixed solution of methanol and tetrahydrofuran.
Further, the surfactant is one or a mixture of more of cetyl trimethyl ammonium bromide, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, span, tween and polyvinylpyrrolidone.
Further, the fluorescence indicator is one or more of PtOEP, ptOEPK or PtTFPP platinum porphyrin complexes, tris (2, 2' -bipyridyl) ruthenium (II) complexes, tris (1, 10-o-phenanthroline) ruthenium (II) complexes, tris (4.7-diphenyl-1.10-o-phenanthroline) ruthenium (II) complexes or tris (5-amino-1, 10-o-phenanthroline) ruthenium (II).
Further, in the S2 step, the ZIF-8 composite coated with the fluorescent indicator is dissolved in an organic solution together with the polymer matrix to form a fluorescent layer mixed solution.
Further, in the ZIF-8 composite material coated with the fluorescent indicator, the molar ratio of the ZIF-8 material to the fluorescent indicator is 10000:1 to 15; in the fluorescent layer, the mass ratio of the ZIF-8 composite material coated with the fluorescent indicator to the polymer matrix is 1.
Further, in forming the light-shielding breathable layer, the method includes: and uniformly mixing the shading breathable layer raw material with a curing agent, adding shading pigment, uniformly stirring to form a shading breathable layer mixture, coating the shading breathable layer mixture on one side of the fluorescent layer far away from the substrate, and curing to form the shading breathable layer.
The invention also provides an oxygen sensor fluorescent film which is manufactured by the manufacturing method of the oxygen sensor fluorescent film.
The invention also provides an oxygen sensor which comprises the oxygen sensor fluorescent film.
In the present invention, a fluorescent indicator is coated in a ZIF-8 material to form a ZIF-8 composite coated with the fluorescent indicator, and then the composite is dispersed in a fluorescent layer. Because the ZIF-8 material has a porous structure, the fluorescent indicator can be easily coated in the ZIF-8, so that the fluorescent indicator can be prevented from being aggregated in the fluorescent layer, and the uniformity of the fluorescent indicator in the fluorescent layer is improved; furthermore, the porous structure of ZIF-8 is combined with the pores of the polymer matrix to form a gas diffusion channel, so that the gas permeability of the membrane is enhanced. Therefore, the oxygen sensor fluorescent film can effectively improve the dispersion of the fluorescent indicator in the polymer matrix and ensure the uniformity in the fluorescent layer; on the other hand, the oxygen sensor fluorescent film has high air permeability due to the synergistic effect of the ZIF-8 and the polymer matrix, so that the sensitivity and the response time of oxygen are improved.
Furthermore, the light-shielding pigment is added into the light-shielding breathable layer, so that the interference of other optical signals and pollutants is prevented while oxygen transmission is ensured, the thickness of the protective layer can be controlled by coating the film with a four-side film coating instrument, and the thin protective layer is prepared to reduce the thickness of the oxygen sensing film. The oxygen sensing film is thin in thickness and small in size, and is favorable for being further applied to miniaturized oxygen detection devices, the perfect protection structure can prevent water and pollution, the difference between every two sensing films is small, and the measuring precision of the oxygen sensor is not influenced even if the films are replaced at any time. The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following preferred embodiments are specifically described below with reference to the accompanying drawings.
Drawings
Fig. 1 is a schematic flow chart illustrating steps of a method for manufacturing an oxygen sensor fluorescent layer according to an embodiment of the present invention.
FIG. 2 shows the phase change of the oxygen sensor fluorescent film after the ZIF-8 material and the fluorescent indicator with different components are added into the oxygen sensor fluorescent film provided by the invention.
FIG. 3 shows the effect on the performance of the oxygen sensor phosphor film at different composite to polymer matrix mass ratios at a molar ratio of ZIF-8 material to fluorescent indicator of 10000.
Fig. 4 is a schematic structural diagram of a fluorescent film of an oxygen sensor according to an embodiment of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description is given with reference to the accompanying drawings and preferred embodiments.
The invention provides a method for manufacturing an oxygen sensor fluorescent film, the oxygen sensor fluorescent film and an oxygen sensor.
Fig. 1 is a schematic flow chart illustrating steps of a method for manufacturing an oxygen sensor fluorescent layer according to an embodiment of the present invention, and as shown in fig. 1, the method for manufacturing an oxygen sensor fluorescent layer includes the following steps:
s1: coating a fluorescent indicator in a ZIF-8 (zeolitic imidazolate framework) material to obtain a ZIF-8 composite material coated with the fluorescent indicator;
in the step, 0.1-0.4 mol of zinc nitrate hexahydrate can be dissolved in 50-200 ml of A solution, such as methanol solution, and then 1-10% of surfactant by mass fraction is added for complete dissolution, so as to obtain the A solution containing zinc ions; and dissolving 0.2-2 mol of 2-methylimidazole and 0.01-0.06 mmol of fluorescent indicator in the solution B, such as 50-200 ml of mixed solution of methanol and tetrahydrofuran, preferably, the volume ratio of methanol to tetrahydrofuran is 1;
slowly adding the solution A into the solution B, stirring by magnetic force, reacting for 24 hours, centrifuging the reacted solution in a centrifuge at the rotating speed of 4000-10000 rpm for 30 minutes to obtain a precipitate, washing the precipitate three times by using methanol, and drying in vacuum at 60 ℃ for 10 hours to obtain the ZIF-8 composite material coated with the fluorescent indicator.
The fluorescence indicator can be one or more of PtOEP, ptOEPK or PtTFPP platinum porphyrin complexes, tris (2, 2' -bipyridyl) ruthenium (II) complexes, tris (1, 10-o-phenanthroline) ruthenium (II) complexes, tris (4.7-diphenyl-1.10-o-phenanthroline) ruthenium (II) complexes, tris (5-amino-1, 10-o-phenanthroline) ruthenium (II) and the like.
The surfactant can be one or more of CTAB (cetyl trimethyl ammonium bromide), P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer), span, tween, polyvinylpyrrolidone (PVP), etc.
Further, the pore size of the ZIF-8 is 2-50nm.
S2: preparing a fluorescent layer mixed solution, wherein the fluorescent layer solution contains a ZIF-8 composite material coated with a fluorescent indicator;
specifically, the ZIF-8 composite coated with the fluorescent indicator and the polymer matrix may be dissolved in an organic solution to form a fluorescent layer mixed solution. Wherein the concentration of the fluorescent indicator in the fluorescent layer mixed solution is 1-10 mg/ml, and the fluorescent indicator is dispersed by shearing and stirring at the rotating speed of 3000-10000 rpm for 0.5-4 h.
More specifically, the molar ratio of ZIF-8 to the fluorescent indicator is 10000; the mass ratio of the ZIF-8 composite material coated with the fluorescent indicator to the polymer matrix is 1.
Further, the polymer matrix may be one or more of Polydimethylsiloxane (PDMS), MQ resin, silicone gel, polystyrene, cellulose derivatives, polytrifluoropropylmethylsiloxane, or polytrimethylsilicon-1-propyne, and the like.
S3: providing a substrate, and solidifying the fluorescent layer mixed solution on the substrate to form a fluorescent layer on the substrate;
in this step, the phosphor layer mixed solution may be drawn down onto the substrate using an automatic drawing down apparatus while being heated, and finally, cured at room temperature to form a phosphor layer on the substrate.
The thickness of the substrate may be 50-300 μm; the thickness of the fluorescent layer may be 10-200 μm.
S4: and forming a light-shielding and air-permeable layer on one side of the fluorescent layer far away from the substrate to form the oxygen sensor fluorescent film.
In the step, after uniformly mixing the shading breathable layer raw material and the curing agent, adding shading pigment and uniformly stirring to form a shading breathable layer mixture, uniformly stirring the shading breathable layer mixture, coating the shading breathable layer mixture on one side of the fluorescent layer far away from the substrate by using a four-side coating instrument, and curing to form the shading breathable layer on the fluorescent layer.
Wherein, the thickness of the shading breathable layer is 10-100 μm, the curing temperature is 50-150 ℃, and the curing time can be 2-48h. The mass ratio of the shading and ventilating layer raw material to the curing agent is 1.1-1, and the shading pigment accounts for 0.1-5% of the mixture of the shading and ventilating layer.
Wherein, the shading breathable layer can be made of polydimethylsiloxane; the opacifying pigment may be carbon black or a white colorant.
In the present invention, a fluorescent indicator is coated in a ZIF-8 material to form a ZIF-8 composite coated with the fluorescent indicator, and then the composite is dispersed in a fluorescent layer. Because the ZIF-8 material has a porous structure, the fluorescent indicator can be easily coated in the ZIF-8, so that the fluorescent indicator can be prevented from being aggregated in the fluorescent layer, and the uniformity of the fluorescent indicator in the fluorescent layer is improved; furthermore, the porous structure of ZIF-8 is combined with the pores of the polymer matrix to form a gas diffusion channel, thereby enhancing the gas permeability of the membrane. Therefore, the oxygen sensor fluorescent film can effectively improve the dispersion of the fluorescent indicator in the polymer matrix and ensure the uniformity in the fluorescent layer; on the other hand, the oxygen sensor fluorescent film has higher air permeability due to the synergistic effect of the ZIF-8 and the polymer matrix, so that the sensitivity to oxygen and the response time are improved.
Furthermore, the light-shielding pigment is added into the light-shielding breathable layer, so that the interference of other optical signals and pollutants is prevented while oxygen transmission is ensured, the thickness of the protective layer can be controlled by coating with a four-side coating instrument, and the thin protective layer is prepared to reduce the thickness of the oxygen sensing film. The oxygen sensing membrane is thin in thickness and small in size, and is favorable for being further applied to miniaturized oxygen detection devices, the perfect protection structure can prevent water and pollution, the difference between every two sensing membranes is small, and the membrane is replaced at any time without influencing the measurement precision of the oxygen sensor.
FIG. 2 shows the phase change of the oxygen sensor fluorescent film after the ZIF-8 material and the fluorescent indicator with different components are added into the oxygen sensor fluorescent film provided by the invention.
As shown in fig. 2, the solvent is toluene, the polymer matrix is MQ resin, the fluorescent indicator is tris (2, 2' -bipyridyl) ruthenium (ii) complex, and the mass ratio of the composite material to the polymer matrix is 1:300 for example, the molar ratio of the ZIF-8 material (indicated by a in FIG. 2) to the fluorescent indicator (indicated by b in FIG. 2) is changed, and the fluorescence in different oxygen sensor fluorescent films is measured by a phase method, so as to obtain the total phase of different nano-micron particles at different times.
As can be seen from fig. 2, since the initial phases of the samples in the air are consistent and the time for reaching the highest phase is almost the same during the measurement, the total phase reflects the phase change in the same time, and the change value is large, so that the measurement is relatively sensitive.
Further, since each sample is from the atmospheric oxygen concentration to the oxygen-free concentration, the phase difference is large, the more precisely each oxygen concentration is corresponded.
Therefore, it can be seen from fig. 2 that the total phase of the oxygen sensor fluorescent film manufactured by the method of the present application reflects a large excellent performance.
FIG. 3 shows the effect on the performance of the oxygen sensor phosphor film at different composite to polymer matrix mass ratios at a molar ratio of ZIF-8 material to fluorescent indicator of 10000.
As can be seen from FIG. 3, the larger the ratio of the ZIF-8 composite (denoted by c in FIG. 3) coated with the fluorescent indicator to the polymer matrix (denoted by d in FIG. 3), the more excellent the performance.
Fig. 4 is a schematic structural diagram of an oxygen sensor fluorescent film according to an embodiment of the present invention. As shown in fig. 4, the present invention also provides an oxidation sensor fluorescent film manufactured by the method for manufacturing an oxidation sensor fluorescent film.
Specifically, the oxygen sensor fluorescent film comprises a substrate 10, a fluorescent layer 20 and a shading breathable layer 30 which are sequentially stacked, wherein the fluorescent layer 20 comprises a polymer matrix, a fluorescent indicator and nano-micro particles.
The invention also provides an oxygen sensor, which comprises the oxygen sensor fluorescent film, and other technical characteristics of the oxygen sensor are referred to in the prior art and are not repeated herein.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for manufacturing an oxygen sensor fluorescent film is characterized in that: the method comprises the following steps:
s1: coating a fluorescent indicator in a ZIF-8 material to obtain a ZIF-8 composite material coated with the fluorescent indicator;
s2: preparing a fluorescent layer mixed solution, wherein the fluorescent layer mixed solution contains a ZIF-8 composite material coated with a fluorescent indicator;
s3: providing a substrate, and solidifying the fluorescent layer mixed solution on the substrate to form a fluorescent layer on the substrate;
s4: and forming a light-shading breathable layer on one side of the fluorescent layer, which is far away from the substrate.
2. The method for manufacturing an oxygen sensor phosphor film according to claim 1, wherein: in forming the fluorescent indicator coated ZIF-8 composite, the method further comprises:
dissolving zinc nitrate hexahydrate in the solution A, and adding a surfactant to obtain a solution A containing zinc ions; dissolving 2-methylimidazole and a fluorescent indicator in the solution B to obtain a solution B containing the fluorescent indicator and 2-methylimidazole;
and mixing the solution A and the solution B, and stirring, centrifuging and drying to obtain the ZIF-8 composite material coated with the fluorescent indicator.
3. The method for manufacturing an oxygen sensor phosphor film according to claim 2, wherein: the solution A is a methanol solution, and the solution B is a mixed solution of methanol and tetrahydrofuran.
4. The method for manufacturing an oxygen sensor phosphor film according to claim 1, wherein: the surfactant is one or a mixture of more of cetyl trimethyl ammonium bromide, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, span, tween and polyvinylpyrrolidone.
5. The method for manufacturing an oxygen sensor phosphor film according to claim 1, wherein: the fluorescence indicator is one or more of PtOEP, ptOEPK or PtTFPP platinum porphyrin complexes, tris (2, 2' -bipyridyl) ruthenium (II) complexes, tris (1, 10-o-phenanthroline) ruthenium (II) complexes, tris (4.7-diphenyl-1.10-o-phenanthroline) ruthenium (II) complexes or tris (5-amino-1, 10-o-phenanthroline) ruthenium (II).
6. The method for manufacturing an oxygen sensor phosphor film according to claim 1, wherein: in the S2 step, the ZIF-8 composite coated with the fluorescent indicator and the polymer matrix are dissolved together in an organic solution to form a fluorescent layer mixed solution.
7. The method for manufacturing an oxygen sensor phosphor film according to claim 6, wherein: in the ZIF-8 composite material coated with the fluorescent indicator, the molar ratio of the ZIF-8 material to the fluorescent indicator is 10000:1 to 15; in the fluorescent layer, the mass ratio of the ZIF-8 composite material coated with the fluorescent indicator to the polymer matrix is 1.
8. The method for manufacturing an oxygen sensor phosphor film according to claim 1, wherein: in forming the light-blocking breathable layer, the method includes: and uniformly mixing the shading breathable layer raw material with a curing agent, adding shading pigment, uniformly stirring to form a shading breathable layer mixture, coating the shading breathable layer mixture on one side of the fluorescent layer far away from the substrate, and curing to form the shading breathable layer.
9. An oxygen sensor fluorescent film characterized in that: the method for manufacturing an oxygen sensor phosphor film according to any one of claims 1 to 8.
10. An oxygen sensor, characterized by: comprising the oxygen sensor fluorescent film according to claim 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211330204.2A CN115575372A (en) | 2022-10-27 | 2022-10-27 | Method for manufacturing oxygen sensor fluorescent film, oxygen sensor fluorescent film and oxygen sensor |
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| CN202211330204.2A CN115575372A (en) | 2022-10-27 | 2022-10-27 | Method for manufacturing oxygen sensor fluorescent film, oxygen sensor fluorescent film and oxygen sensor |
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