CN116990268A - Optical oxygen sensing film for optical oxygen sensor and preparation method thereof - Google Patents
Optical oxygen sensing film for optical oxygen sensor and preparation method thereof Download PDFInfo
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- 239000001301 oxygen Substances 0.000 title claims abstract description 155
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 155
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 230000003287 optical effect Effects 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims description 21
- 239000002245 particle Substances 0.000 claims abstract description 34
- 239000006229 carbon black Substances 0.000 claims abstract description 19
- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 claims abstract description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 15
- 239000010949 copper Substances 0.000 claims abstract description 15
- 238000002955 isolation Methods 0.000 claims abstract description 12
- 229920000642 polymer Polymers 0.000 claims abstract description 11
- 230000035699 permeability Effects 0.000 claims abstract description 7
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 27
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 27
- -1 polydimethylsiloxane Polymers 0.000 claims description 27
- 239000011550 stock solution Substances 0.000 claims description 23
- 239000012528 membrane Substances 0.000 claims description 21
- 238000004528 spin coating Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 7
- 238000010907 mechanical stirring Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 229910001369 Brass Inorganic materials 0.000 claims description 6
- 239000010951 brass Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- VFMUXPQZKOKPOF-UHFFFAOYSA-N 2,3,7,8,12,13,17,18-octaethyl-21,23-dihydroporphyrin platinum Chemical compound [Pt].CCc1c(CC)c2cc3[nH]c(cc4nc(cc5[nH]c(cc1n2)c(CC)c5CC)c(CC)c4CC)c(CC)c3CC VFMUXPQZKOKPOF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 239000012327 Ruthenium complex Substances 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000003892 spreading Methods 0.000 claims description 2
- 230000007480 spreading Effects 0.000 claims description 2
- 230000004044 response Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 3
- 230000001954 sterilising effect Effects 0.000 abstract description 3
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000012216 screening Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 230000007774 longterm Effects 0.000 description 4
- 238000012423 maintenance Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000005273 aeration Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000027734 detection of oxygen Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000010071 organism adhesion Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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"
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Immunology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention provides an optical oxygen sensing film for an optical oxygen sensor, which is formed by compounding an oxygen sensitive fluorescent film and a light isolating film; the oxygen sensitive fluorescent film is composed of oxygen sensitive fluorescein and a high oxygen permeability polymer carrier; the light isolation film is composed of anti-biological pollution particles, carbon black particles and a high oxygen-permeable polymer carrier. According to the invention, copper with sterilization effect is directly integrated in the oxygen sensing film, instead of making the copper into a net shape or screening shape to be arranged at the front end of the film, and the problems of response speed reduction and the like caused by blockage of a net-shaped protective cover can be effectively avoided.
Description
Technical Field
The invention belongs to the technical field of oxygen detection, and particularly relates to a preparation method of an anti-biological pollution optical oxygen sensing film.
Background
Oxygen is a key substance for maintaining vital activity, so accurate detection of oxygen content is critical for life safety. In the past, a number of sensing techniques have been developed for detecting oxygen content in the gas and liquid phases. The optical sensing technology based on the fluorescence quenching principle is widely focused and applied to the on-line detection of oxygen due to the characteristics of no consumption of oxygen, strong anti-interference performance, high response speed, no maintenance and the like. The oxygen sensing film is a core element of an optical oxygen sensor, and is a key factor for determining the performances of the sensor, such as sensitivity, response speed, stability, service life and the like.
In biochemical applications such as sewage treatment, aquaculture, etc., optical oxygen sensors often suffer from serious biological contamination problems.
Biological pollution refers to the phenomenon that organisms in a measuring medium adhere to the surface of an oxygen sensing film, so that the response speed and the measuring accuracy of a sensor are obviously reduced.
In order to relieve biological pollution, the prior solution comprises periodic manual cleaning of an optical oxygen sensing film, automatic cleaning of the oxygen sensing film by mechanical hanging brushing, addition of a copper mesh protective cover at the front end of the oxygen sensing film, and the like. However, these methods introduce additional new problems during application, such as increased maintenance effort, damage to the oxygen sensing membrane, clogging of the copper mesh shield, etc. In order to reduce maintenance workload and use of anti-pollution auxiliary components, it is necessary to develop an anti-biological pollution type oxygen sensing membrane so as to realize long-term stable monitoring of oxygen in biochemical application scenes.
Disclosure of Invention
The invention aims to develop an anti-biological pollution optical oxygen sensing film and a preparation method thereof.
The technical scheme provided by the invention is as follows: an optical oxygen sensing film for an optical oxygen sensor is formed by compounding an oxygen sensitive fluorescent film and an optical isolation film;
the oxygen sensitive fluorescent film is composed of oxygen sensitive fluorescein and a high oxygen permeability polymer carrier;
the light isolation film is composed of anti-biological pollution particles, carbon black particles and a high oxygen-permeable polymer carrier.
Further, the oxygen-sensitive fluorescein is a metal ruthenium complex and a platinum complex.
Preferably, the oxygen-sensitive fluorescein is platinum octaethylporphyrin.
Further, the high oxygen permeability polymer carrier is one or more of polydimethylsiloxane, polymethyl methacrylate cellulose derivative, polystyrene and fluorinated copolymer.
Preferably, the high oxygen permeable polymer carrier is polydimethylsiloxane.
Further, the above-mentioned anti-biological pollution particles are 2 microns of brass powder;
preferably, the carbon black particles are 2 microns.
A preparation method of an optical oxygen sensing film for an optical oxygen sensor,
the optical oxygen sensing film consists of a light isolation film and an oxygen sensitive fluorescent film;
the light isolation film is composed of carbon black particles, anti-biological pollution copper particles and a high oxygen-permeable polydimethylsiloxane carrier;
the oxygen sensitive fluorescent film is composed of a high oxygen permeability polydimethylsiloxane carrier and oxygen sensitive fluorescein;
the preparation steps of the optical oxygen sensing film are as follows;
(S1) preparation of oxygen-sensitive fluorescent film stock solution: weighing polydimethylsiloxane carrier and oxygen-sensitive fluorescein, fully mixing the polydimethylsiloxane carrier and the oxygen-sensitive fluorescein by a mechanical stirring mode, and standing for defoaming to obtain oxygen-sensitive fluorescent film stock solution;
(S2) preparation of an oxygen-sensitive fluorescent film: coating the oxygen sensitive fluorescent film stock solution on a glass plate in a spin coating mode, wherein the spin coating rotating speed is 500rpm, and the spin coating time is 3min; after coating, placing the glass plate in a baking oven at 100 ℃ for baking for 30 min, and curing to obtain an oxygen-sensitive fluorescent film;
(S3) preparation of a shading film stock solution: weighing a certain amount of polydimethylsiloxane carrier, carbon black particles and brass particles, fully mixing the carrier with the carbon black and copper particles in a mechanical stirring mode, and standing for defoaming to obtain a shading film stock solution;
(S4) preparation of an optical oxygen sensing film: spreading the light shielding film stock solution prepared in the step 3 on the oxygen sensitive fluorescent film prepared in the step 2, uniformly covering the stock solution on the surface of the fluorescent film in a spin coating mode, wherein the spin coating rotating speed is 200rpm, the spin coating time is 3min, and after the coating is finished, placing the fluorescent film in a baking oven at 100 ℃ for baking for 30 min, and curing the polydimethylsiloxane carrier to obtain the optical oxygen sensing film with a double-layer structure.
The mass ratio of the optical polydimethylsiloxane carrier to the oxygen-sensitive fluorescein is 100:1.
The mass ratio of the optical polydimethylsiloxane carrier to the carbon black particles to the brass particles is 5:2:1.
The invention prepares the oxygen sensing film for preventing organism adhesion (resisting biological pollution) by doping micron copper particles with sterilization effect in the oxygen sensing film, and the film has the following advantages:
(1) No other auxiliary components (such as mechanical hanging brushes) for resisting biological pollution are needed, so that the structure of the sensor is simplified, and the oxygen sensing membrane is not damaged.
(2) Copper with sterilization effect is directly integrated in the oxygen sensing membrane instead of being made into a net shape or a screen shape and placed at the front end of the membrane, so that the problems of response speed reduction and the like caused by blockage of a net-shaped protective cover can be effectively avoided;
(3) The copper microparticles are embedded in a highly oxygen permeable polymer carrier and do not leak into the environment, causing environmental risks (biotoxicity).
(4) The structure of the sensor is simplified, and the manufacturing and maintenance cost of the sensor is reduced.
Drawings
FIG. 1 is a schematic diagram of the structure of an anti-biofouling optical oxygen sensor film in example 1;
FIG. 2 is a comparison of anti-biofouling oxygen sensor membrane versus oxygen sensor membrane DO detection performance without anti-biofouling function;
FIG. 3 shows long-term comparative test results of DO sensor stuck with anti-biofouling membrane and without anti-biofouling membrane in a wastewater aeration tank;
1-a light isolation film; 2-oxygen sensitive fluorescent film; 3-a highly oxygen permeable polymeric carrier; 4-carbon black particles; 5-anti-biocontamination copper particles; 6-oxygen sensitive fluorescein.
A-an output curve of the DO sensor stuck with the anti-biological pollution type oxygen sensing film; b-output curve of DO sensor with or without anti-biofouling oxygen sensor film.
Detailed Description
The invention will be further illustrated with reference to the following specific examples, but the invention is not limited to the following examples. The methods are conventional methods unless otherwise specified. The starting materials are available from published commercial sources unless otherwise specified.
Example 1 preparation of optical oxygen sensing film
As shown in FIG. 1, the anti-biological pollution optical oxygen sensing film provided by the invention is formed by compounding a light isolation film 1 and an oxygen sensitive fluorescent film 2. The light isolation film is composed of carbon black particles 4, anti-biological pollution copper particles 5 and a high oxygen-permeable polydimethylsiloxane carrier 3; the oxygen sensitive fluorescent film is composed of a high oxygen permeability polydimethylsiloxane carrier 3 and oxygen sensitive fluorescein 6. The specific preparation method of the oxygen sensing membrane is as follows;
(1) Preparing oxygen sensitive fluorescent film stock solution: weighing 5 g of polydimethylsiloxane carrier 3 (dakangnin 184, main agent: curing agent=10:1) and 0.05 g of oxygen-sensitive fluorescein 6 (platinum octaethylporphyrin purchased from sigma reagent net), fully mixing the carrier and the oxygen-sensitive fluorescein by a mechanical stirring mode, and standing for defoaming to obtain an oxygen-sensitive fluorescent film stock solution;
(2) Preparing an oxygen sensitive fluorescent film: the oxygen sensitive fluorescent film stock solution is coated on a glass plate in a spin coating mode, the spin coating rotating speed is 500rpm, and the spin coating time is 3min. After coating, placing the glass plate in a baking oven at 100 ℃ for 30 min, and curing the polydimethylsiloxane carrier to obtain an oxygen-sensitive fluorescent film;
(3) Preparation of a shading film stock solution without an anti-biological pollution function: weighing 5 g of polydimethylsiloxane carrier 3 and 2 g of carbon black particles, fully mixing the carrier and the carbon black particles in a mechanical stirring mode, and standing for defoaming to obtain a shading film stock solution;
(4) Preparation of a shading film stock solution with an anti-biological pollution function: weighing 5 g of polydimethylsiloxane carrier, 2 g of carbon black particles 4 and 1 g of copper particles, fully mixing the carrier with the carbon black and the copper particles in a mechanical stirring mode, and standing for defoaming to obtain a shading film stock solution;
(5) Preparation of an oxygen sensing film: and (3) flatly paving the shading film stock solution prepared in the steps (3) and (4) on the oxygen-sensitive fluorescent film prepared in the step (2), and uniformly covering the stock solution on the surface of the fluorescent film in a spin coating mode, wherein the spin coating rotating speed is 200rpm, and the spin coating time is 3min. And after the coating is finished, placing the film in a baking oven at 100 ℃ for baking for 30 min, and obtaining the optical oxygen sensing film with a double-layer structure after the polydimethylsiloxane carrier is solidified, wherein the optical oxygen sensing film comprises an anti-biological pollution oxygen sensing film and an oxygen sensing film without an anti-biological pollution function.
Example 2 comparison of anti-biofouling oxygen sensor Membrane with oxygen sensor Membrane Dissolved Oxygen (DO) detection Performance without anti-biofouling function
The anti-biofouling oxygen sensing membrane and the oxygen sensing membrane without the anti-biofouling function provided in the example 1 are respectively stuck on the membrane caps of the two DO sensors, and the phase difference values under different dissolved oxygen concentrations are measured according to the following steps, so that a DO detection signal response curve is drawn.
(1) A glass beaker with a capacity of 1L and containing 500ml of purified water is placed in a constant temperature water bath with a temperature of 20 ℃;
(2) Continuously exposing oxygen standard gas (Chinese standard substance net) with oxygen saturation within the range of 0-100% to the step 1 to prepare DO standard solutions with different concentrations;
(3) Placing the DO sensor in a beaker, continuously aerating, and recording a phase Difference (DP) signal value of the sensor after the sensor shows stable value;
(4) And drawing a DO detection signal response curve by using the DO concentration value and the corresponding measured phase difference signal value. Based on the signal response curve, evaluating detection performances of different oxygen sensing films;
(5) The measurement result shows that with the increase of DO concentration, the phase difference of the anti-biological pollution oxygen sensing film and the oxygen sensing film without the anti-biological pollution function is gradually reduced, and the obvious proportional relationship is presented, so that the oxygen sensing film can be used for quantitative detection of DO. In addition, the signal variation ranges of the two membranes are equivalent, which shows that the anti-biological pollution oxygen sensing membrane and the oxygen sensing membrane without the anti-biological pollution function have no obvious difference in DO detection performance.
Example 3, in situ comparative testing of anti-biofouling oxygen sensing Membrane and oxygen sensing Membrane without anti-biofouling function
The anti-biological pollution oxygen sensing film and the oxygen sensing film without the anti-biological pollution function provided in the embodiment 1 are respectively stuck on the optical DO sensor, the sensors are bound together, and the oxygen sensing film are placed in a sewage aeration tank for long-term comparison test, and the specific method is as follows:
(1) The DO sensor stuck with the anti-biological pollution sensor film and the oxygen sensor film without the anti-biological pollution function is arranged in an aeration tank of a sewage treatment plant, and the film surfaces of the sensor are kept on the same horizontal line (so as to prevent the uneven distribution of the oxygen concentration in the solution from influencing the comparison test result).
(2) Transmitting back real-time measurement data of the oxygen sensor by using 4G RTU wireless transmission equipment, and drawing a real-time curve according to the measurement data;
(3) Comparing real-time measurement curves of the DO sensor adhered with the anti-biological pollution oxygen sensing film and the oxygen sensing film without the anti-biological pollution function, and evaluating measurement performances of the two films in actual biochemical application scenes;
(4) The comparison of the real-time measurement curves shows that the measurement values of the DO sensor, which is stuck with the anti-biological pollution oxygen sensing film (the output test curve is A) and the oxygen sensing film without the anti-biological pollution function (the output test curve is B), are almost consistent (the curves A and B almost coincide before the vertical dotted line) at the beginning of the comparison test (when both films are not attached with organisms), which indicates that both the sensors can generate quick response to the change of DO concentration; along with the extension between the comparison tests (microorganisms are gradually attached to the oxygen sensing films), the response speed of the DO sensor attached with the oxygen sensing film with the function of resisting biological pollution to the change of the oxygen concentration is gradually slowed down, and the response speed is obviously slower than that of the DO sensor attached with the oxygen sensing film with the function of resisting biological pollution (after vertical dotted lines, the curves A and B are not overlapped). The result shows that the anti-biological pollution type oxygen sensing film developed by the invention can effectively weaken the adhesion of microorganisms on the film surface, thereby guaranteeing the long-term stability, accuracy and response speed of the optical oxygen sensor in biochemical application scenes.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
Claims (10)
1. An optical oxygen sensing film for an optical oxygen sensor is characterized by being formed by combining an oxygen sensitive fluorescent film and an optical isolation film;
the oxygen-sensitive fluorescent film consists of oxygen-sensitive fluorescein and a high oxygen-permeable polymer carrier;
the light isolation film is composed of anti-biological pollution particles, carbon black particles and a high oxygen permeability polymer carrier.
2. The optical oxygen sensing film of claim 1, wherein the oxygen sensitive fluorescein is a metallic ruthenium complex, a platinum complex.
3. The optical oxygen sensing film of claim 1, wherein the oxygen-sensitive fluorescein is platinum octaethylporphyrin.
4. The optical oxygen sensing film of claim 1, wherein the high oxygen permeability polymer carrier is one or more of polydimethylsiloxane, polymethyl methacrylate cellulose derivative, polystyrene, fluorinated copolymer.
5. The optical oxygen sensing film of claim 1, wherein the high oxygen permeable polymer carrier is polydimethylsiloxane.
6. The optical oxygen sensing film of claim 1, wherein the anti-biofouling particles are 2 microns of brass powder.
7. The optical oxygen sensing film of claim 1, wherein the carbon black particles are 2 microns.
8. A preparation method of an optical oxygen sensing film for an optical oxygen sensor is characterized in that,
the optical oxygen sensing film consists of a light isolation film and an oxygen sensitive fluorescent film;
the light isolation film consists of carbon black particles, anti-biological pollution copper particles and a high oxygen-permeable polydimethylsiloxane carrier;
the oxygen-sensitive fluorescent film consists of a high oxygen-permeable polydimethylsiloxane carrier 3 and oxygen-sensitive fluorescein 6;
the preparation steps of the optical oxygen sensing film are as follows;
(S1) preparation of oxygen-sensitive fluorescent film stock solution: weighing polydimethylsiloxane carrier and oxygen-sensitive fluorescein, fully mixing the polydimethylsiloxane carrier and the oxygen-sensitive fluorescein by a mechanical stirring mode, and standing for defoaming to obtain oxygen-sensitive fluorescent film stock solution;
(S2) preparation of an oxygen-sensitive fluorescent film: coating the oxygen sensitive fluorescent film stock solution on a glass plate in a spin coating mode, wherein the spin coating rotating speed is 500rpm, and the spin coating time is 3min; after coating, placing the glass plate in a baking oven at 100 ℃ for baking for 30 min, and curing to obtain an oxygen-sensitive fluorescent film;
(S3) preparation of a shading film stock solution: weighing a certain amount of polydimethylsiloxane carrier, carbon black particles and brass particles, fully mixing the carrier with the carbon black and copper particles in a mechanical stirring mode, and standing for defoaming to obtain a shading film stock solution;
(S4) preparation of an oxygen sensing membrane: spreading the light shielding film stock solution prepared in the step 3 on the oxygen sensitive fluorescent film prepared in the step 2, uniformly covering the stock solution on the surface of the fluorescent film in a spin coating mode, wherein the spin coating rotating speed is 200rpm, the spin coating time is 3min, and after the coating is finished, placing the fluorescent film in a baking oven at 100 ℃ for baking for 30 min, and curing the polydimethylsiloxane carrier to obtain the optical oxygen sensing film with a double-layer structure.
9. The method of claim 8, wherein the mass ratio of polydimethylsiloxane carrier to oxygen-sensitive fluorescein is 100:1.
10. the method of claim 8, wherein the mass ratio of polydimethylsiloxane carrier, carbon black particles, and brass particles is 5:2:1.
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| CN202310726341.6A CN116990268A (en) | 2023-06-19 | 2023-06-19 | Optical oxygen sensing film for optical oxygen sensor and preparation method thereof |
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| CN202310726341.6A CN116990268A (en) | 2023-06-19 | 2023-06-19 | Optical oxygen sensing film for optical oxygen sensor and preparation method thereof |
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