CN114324285A - Optical oxygen sensing membrane and preparation method and application thereof - Google Patents
Optical oxygen sensing membrane and preparation method and application thereof Download PDFInfo
- Publication number
- CN114324285A CN114324285A CN202210011315.0A CN202210011315A CN114324285A CN 114324285 A CN114324285 A CN 114324285A CN 202210011315 A CN202210011315 A CN 202210011315A CN 114324285 A CN114324285 A CN 114324285A
- Authority
- CN
- China
- Prior art keywords
- oxygen sensing
- fluorescent
- sensing film
- chip layer
- membrane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to the technical field of oxygen sensing detection, in particular to an optical oxygen sensing membrane and a preparation method and application thereof. The optical oxygen sensing film sheet comprises a fluorescent oxygen sensing film layer and a chip layer, wherein the fluorescent oxygen sensing film layer is adhered to the upper surface of the chip layer; the fluorescent oxygen sensing film includes a polymer matrix and a fluorescent indicator uniformly dispersed in the polymer matrix. The optical oxygen sensing membrane sheet provided by the invention integrates the microfluidic channel and the optical oxygen sensing membrane, can sensitively and quickly respond to gaseous oxygen and dissolved oxygen, and can improve the detection accuracy by double-channel detection; the chip layer is manufactured by adopting a 3D printing technology, and the manufacturing process is simple, good in air tightness, small in size, convenient to carry and capable of being repeatedly used.
Description
Technical Field
The invention relates to the technical field of oxygen sensing detection, in particular to an optical oxygen sensing membrane and a preparation method and application thereof.
Background
The detection of oxygen is vital to biomedicine and water environment monitoring, a diver needs to carry a respirator during underwater operation, the oxygen partial pressure in the respirator can be increased along with the increase of diving depth, and oxygen deficiency or oxygen poisoning is likely to occur if the diver cannot timely detect and take corresponding measures after abnormal air supply, so that the life safety of people is directly endangered. In order to ensure the safety of the respiratory system of underwater operators, the oxygen content in the respirator needs to be effectively monitored in real time. The detection of the dissolved oxygen in water has very important significance for the fields of environmental monitoring, aquaculture and the like.
The sensor technology attracts wide attention as a high and new technology recognized at home and abroad, wherein the oxygen sensor is applied to various fields as an important device for monitoring the oxygen content. Currently, there are several foreign oxygen monitoring products, such as the electrochemical UwatecOXY2 scuba respirator from Scubapro, USA, and the optical LuminoXLOX-02 oxygen sensor from Gaslab, which have a long service life but a high cost. The electrochemical oxygen sensor developed by the earliest institute of ship rework 718 in China has low detection limit and small interference, but needs to be calibrated regularly, is greatly influenced by temperature, humidity and pressure, and the storage environment also influences the service life. The optical sensor has strong environment adaptability, rapid and sensitive measurement, light and handy structure and easy carrying, and can be used in toxic and strong radiation environments, thereby having wide application.
The fluorescence method oxygen detection sensor is based on a fluorescence quenching principle, and utilizes the capability of oxygen to dynamically quench emitted light, so that the fluorescence intensity and the fluorescence lifetime of the emitted light are reduced. The key of the fluorescence sensor is a fluorescent film, and the preparation of the fluorescent film mainly relates to the selection and fixation of a fluorescence indicator at present. The commonly used ruthenium complex has stronger fluorescence lifetime and photobleaching resistance, and is an ideal fluorescence indicator. The fluorescent indicator is usually fixed on the membrane carrier by means of physical fixation and chemical fixation, and the membrane carrier is required to have good permeability and mechanical properties.
The microfluidic chip analysis system has the characteristics of easy integration and portability, and provides wide application prospects in the aspects of biomedicine, environmental detection and protection. The micro-fluidic chip is combined with optical detection, so that the detection method widely applied in the field of scientific research is formed.
Disclosure of Invention
The invention aims to provide an optical oxygen sensing membrane and a preparation method and application thereof, and solves the problems that the existing oxygen sensing membrane is complex in process and high in cost, and cannot detect the change of oxygen concentration in a solution and air at the same time.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the present invention provides an optical oxygen sensing film sheet, which includes a fluorescent oxygen sensing film layer and a chip layer, wherein the fluorescent oxygen sensing film layer is adhered to the upper surface of the chip layer; two fluid microchannels which are not communicated are arranged in the chip layer, a sample inlet and a sample outlet are arranged at two ends of each fluid microchannel, and two liquid storage tanks are arranged in the middle of each fluid microchannel.
The fluorescent oxygen sensing film of the present invention comprises a polymer matrix and a fluorescent indicator uniformly embedded in the polymer matrix.
In some embodiments of the present invention, the polymer matrix is selected from one or a combination of polyvinyl alcohol, polyvinyl chloride and polydimethylsiloxane.
In some embodiments of the invention, the fluorescent indicator is selected from any one of tris (2, 2' -bipyridine) ruthenium (ii) complex, tris (1, 10-phenanthroline) ruthenium (ii) complex, tris (4, 7-biphenyl-1, 10-phenanthroline) ruthenium (ii) complex, or tris (5-amino-1, 10-phenanthroline) ruthenium (ii) complex.
A second aspect of the present invention provides a method for producing an optical oxygen sensing film sheet, comprising the steps of:
step one, 3D printing a three-dimensional model of a chip layer to obtain a printing structure, and carrying out ultraviolet curing on the printing structure to obtain the chip layer;
step two, preparing a fluorescent oxygen sensing film layer;
and step three, uniformly coating an ultraviolet curing adhesive on the upper surface of the chip layer, correspondingly adhering the fluorescent oxygen sensing film layer and the upper surface of the chip layer, and curing under ultraviolet light to obtain the optical oxygen sensing film.
In some embodiments of the present invention, the preparing the fluorescent oxygen sensing film layer in the second step specifically includes the following operations:
s1, preparing a fluorescent indicator solution;
s2, preparing a polymer matrix solution;
s3, uniformly mixing the polymer matrix solution with a curing agent to obtain a matrix solution containing the curing agent;
and S4, adding the fluorescent indicator solution into the matrix solution containing the curing agent according to the weight ratio, uniformly mixing to obtain a membrane making solution, removing bubbles in the membrane making solution, introducing the membrane making solution into a reverse mold, heating for curing, and demolding to obtain the fluorescent oxygen sensing membrane layer.
The third aspect of the present invention provides the use of the above optical oxygen sensing film sheet for oxygen sensing detection.
Compared with the prior art, the invention has the following beneficial effects:
1. the fluorescent oxygen sensing film layer provided by the invention can sensitively and quickly respond to molecular oxygen, when oxygen in a gas or liquid sample is diffused to the fluorescent film, the fluorescence is quenched, the quenching degree of the fluorescence is related to the oxygen content, and the fluorescent oxygen sensing film layer has the characteristics of low cost, wide linear range, good response reversibility and long service life.
2. The optical oxygen sensing film provided by the invention adopts epoxy resin to bond the fluorescent oxygen sensing film layer and the 3D printing chip layer, integrates the microfluidic channel and the optical oxygen sensing film into a whole, has high commercialization degree, can accurately control the flow rate of liquid, can detect the concentration of oxygen in the air and dissolved oxygen in the liquid in real time, can improve the detection accuracy by dual-channel detection, can be recycled for multiple times, has no pollution to the environment, has high integration degree, simple manufacturing process, good air tightness, small volume and convenient carrying.
Drawings
Fig. 1 is a schematic cross-sectional view of an optical oxygen sensing membrane according to the present invention.
Fig. 2 is a schematic top view of the optical oxygen sensing film according to the present invention.
FIG. 3 is a schematic cross-sectional view of a reverse mold for a fluorescent oxygen sensor film according to the present invention.
Fig. 4 is a schematic top view of a reverse mold for a fluorescent oxygen sensing film layer according to the present invention.
Fig. 5 is a diagram of an embodiment of the optical oxygen sensing membrane of the present invention.
FIG. 6 is a graph showing the fluorescence intensity detected in air of the optical oxygen sensing membrane of the present invention.
Fig. 7 is a fluorescence lifetime test chart of the optical oxygen sensing membrane sheet of the present invention.
Description of reference numerals: 1-a fluorescent oxygen sensing film layer; 2-a chip layer; 3-a sample inlet; 4, a sample outlet; 5-a fluidic microchannel; 6-detection zone.
Detailed Description
The optical oxygen sensing film of the present invention, and the preparation method and application thereof are described in detail below.
The first aspect of the present invention provides an optical oxygen sensing membrane, the structure of which is shown in fig. 1, fig. 2 and fig. 5, wherein two sides of the upper surface of the optical oxygen sensing membrane are provided with two sample inlets 3 and two sample outlets 4, and the middle part is provided with four detection regions 6; the optical oxygen sensing film comprises an upper fluorescent oxygen sensing film layer 1 and a lower chip layer 2, wherein the fluorescent oxygen sensing film layer 1 is adhered to the upper surface of the chip layer 2; two fluid micro-channels 5 which are not communicated are arranged in the chip layer 1, and a sample inlet 3 and a sample outlet 4 are symmetrically arranged at two ends of each fluid micro-channel 5; two liquid storage tanks are symmetrically arranged at the middle part of each fluid micro-channel.
In some embodiments of the present invention, the two sample inlets 3 and the two sample outlets 4 are symmetrically arranged along the axial center line of the chip layer; the four detection areas 6 are respectively and symmetrically arranged along the axial central line and the radial central line of the chip layer.
In some embodiments of the present invention, as shown in fig. 2 and 5, the two unconnected fluidic microchannels 5 in the chip layer are arranged in parallel, enabling real-time detection of changes in oxygen concentration in solution and gas in different channels.
In some embodiments of the invention, as shown in fig. 5, the reservoir in the chip layer is a cylindrical reservoir.
In some embodiments of the present invention, the chip layer is made of a transparent photosensitive resin material. In some preferred embodiments of the present invention, the transparent photosensitive resin is selected from one or two combinations of transparent photosensitive resins transparent v4 and clear resin v4 of formlabs. High transparency and good mechanical property, and is easy to be further jointed with the fluorescent oxygen sensing film.
The fluorescent oxygen sensing film of the present invention comprises a polymer matrix and a fluorescent indicator uniformly embedded in the polymer matrix.
The fluorescent oxygen sensing film provided by the invention is based on the principle of fluorescence quenching, when oxygen in a gas or liquid sample is diffused to the fluorescent oxygen sensing film, the fluorescence is quenched, and the quenching degree of the fluorescence is related to the oxygen content. The oxygen content to be measured can be calculated by measuring the fluorescence intensity or the fluorescence lifetime of the part, the oxygen content is low when the fluorescence signal is strong, and the oxygen content is high when the fluorescence signal is weak.
The polymer matrix is selected from one or a combination of polyvinyl alcohol, polyvinyl chloride and polydimethylsiloxane; the fluorescent indicator is selected from any one of a tris (2, 2' -bipyridyl) ruthenium (II) complex, a tris (1, 10-phenanthroline) ruthenium (II) complex, a tris (4, 7-biphenyl-1, 10-phenanthroline) ruthenium (II) complex or a tris (5-amino-1, 10-phenanthroline) ruthenium (II) complex. The polymer matrix of the invention is selected from one or a combination of more of polyvinyl alcohol, polyvinyl chloride or polydimethylsiloxane matrix materials, so that the fluorescent film matrix has higher oxygen permeability, and is favorable for uniform dispersion of the fluorescent indicator when being combined with a corresponding organic solvent, and the stability of the indicator is improved. The ruthenium (II) complex selected by the fluorescent indicator has the advantages of long excitation life, high quantum yield, good stability, strong sensitivity to oxygen, no oxygen consumption, acid and alkali resistance and high temperature resistance.
A second aspect of the present invention provides a method for producing an optical oxygen sensing film sheet, comprising the steps of:
step one, importing a three-dimensional model file of a chip layer into relevant software of a 3D printer, performing 3D printing to obtain a printing structure, and then performing ultraviolet curing on the printing structure to obtain the chip layer;
step two, preparing a fluorescent oxygen sensing film layer;
and step three, uniformly coating an ultraviolet curing adhesive on the upper surface of the chip layer, correspondingly adhering the fluorescent oxygen sensing film layer and the upper surface of the chip layer, and curing under ultraviolet light to obtain the optical oxygen sensing film.
In some embodiments of the present invention, the software used by the 3D printer in the first step is form.
In some embodiments of the present invention, in step one, a chip layer support structure, a layering thickness, printing material properties, proportioning parameters, etc. are set before printing.
In some embodiments of the present invention, in the first step, the printing structure needs to be soaked in a cleaning solution for 2-4 hours before ultraviolet curing, so as to wash away excess uncured printing material. The cleaning solution is not particularly limited, and the excess uncured printing material can be washed away. In some preferred embodiments of the present invention, the cleaning solution is selected from one or a combination of several of isopropyl alcohol, n-propyl alcohol, acetone, and acetonitrile.
In some embodiments of the present invention, the ultraviolet curing temperature in the first step is 35 to 80 ℃, and the curing time is 3 to 10 hours. In some preferred embodiments of the present invention, the ultraviolet curing temperature in the first step is 35 ℃, and the curing time is 3-5 hours.
In some embodiments of the present invention, the ultraviolet curing temperature in step three is 35 to 80 ℃, and the curing time is 3 to 5 hours. In some preferred embodiments of the present invention, the uv curing temperature in step three is 50 ℃ and the curing time is 4 h.
In some embodiments of the present invention, the uv curable adhesive in step three is an epoxy adhesive.
In some embodiments of the present invention, the structure of the fluorescent oxygen sensing film layer prepared in step two is perfectly matched to the printed structure described in step one.
In some embodiments of the present invention, the step two of preparing the fluorescent oxygen sensing film layer specifically comprises the following operations:
s1, preparing a fluorescent indicator solution;
s2, preparing a polymer matrix solution;
s3, uniformly mixing the polymer matrix solution with a curing agent to obtain a matrix solution containing the curing agent;
and S4, adding the fluorescent indicator solution into the matrix solution containing the curing agent according to the weight ratio, uniformly mixing to obtain a membrane making solution, removing bubbles in the membrane making solution, introducing the membrane making solution into a reverse mold, heating for curing, and demolding to obtain the fluorescent oxygen sensing membrane layer.
In some embodiments of the present invention, the weight ratio of the fluorescent indicator to the organic solvent in the fluorescent indicator solution in S1 is 1: 8-10. In some preferred embodiments of the present invention, the organic solvent is selected from any one of ethanol, toluene, dichloromethane, chloroform, and N, N-dimethylformamide.
In some embodiments of the present invention, the polymer matrix solution in S2 is dow corning 184, the main components being polymer monomers and cross-linking agents; the weight ratio of polymer monomer to crosslinker was 10: 1. The polymer has the advantages of no toxicity, ventilation, elasticity, good light transmittance and good hydrophobicity.
In some embodiments of the invention, the weight ratio of the curing agent to the polymer matrix solution in S3 is 1: 8-10.
In some embodiments of the invention, the weight ratio of the fluorescent indicator solution to the matrix solution containing the curing agent in S4 is 1: 8-10.
In some embodiments of the present invention, the specific operation of removing bubbles in S4 is to place the membrane-forming solution into a vacuum pump for vacuum pumping.
In some embodiments of the present invention, the cross-sectional structure of the reverse mold in S4 is as shown in fig. 3, and the top view structure is as shown in fig. 4, so that the fluorescent oxygen sensing film can be completely matched with the structure of the chip layer, thereby producing the optical oxygen sensing film sheet shown in fig. 1 and 2.
In some embodiments of the present invention, repeated evacuation under vacuum is required to maintain the liquid level before the heat curing in S4.
In some embodiments of the present invention, the heating curing temperature in S4 is 55 to 90 ℃, and the curing time is 3 to 8 hours.
The third aspect of the present invention provides the use of the above optical oxygen sensing film sheet for oxygen sensing detection.
The optical oxygen sensing membrane provided by the invention integrates the microfluidic channel and the optical oxygen sensing membrane, has the advantages of simple structure and convenience in use, can sensitively and quickly respond to gaseous oxygen and dissolved oxygen, and can meet the requirements of modern industry on high sensitivity, high stability and high accuracy of the oxygen sensor.
The following describes the preferred embodiments of the present invention in further detail. When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, and materials used in the examples, any methods, devices, and materials similar or equivalent to those described in the examples herein can be used in the practice of the invention, as would be known to one skilled in the art and the description of the invention.
Example 1: preparation of optical oxygen sensing film
(1) Preparation of the chip layer
Importing the three-dimensional model file into a related software-before of a 3D printer, setting parameters such as a supporting structure, a layering thickness and materials required during 3D printing, and then connecting the three-dimensional model file with the 3D printer for printing; the supporting structure comprises two channels arranged in parallel, 4 detection areas, 2 sample inlets and 2 sample outlets, wherein the two channels are shown in figure 1.
After printing, putting the printing structure into an isopropanol solution to be soaked for 3 hours, and washing away redundant uncured printing materials; and then putting the mixture into an ultraviolet post-curing box for post-curing, wherein the temperature of the curing box is set to be 35 ℃, and the curing time is 3-5 hours.
(2) Preparation of fluorescent oxygen sensing film layer
S1, preparing a fluorescent indicator solution, and dissolving a fluorescent indicator tris (4, 7-biphenyl-1, 10-phenanthroline) ruthenium (II) complex in ethanol according to a ratio of 1: 8-10 (w/w) to prepare a 5mL solution;
s2, preparing 10g of polydimethylsiloxane PDMS solution;
s3, uniformly stirring the polydimethylsiloxane PDMS solution and the curing agent according to a ratio of 10:1(w/w) to obtain a matrix solution containing the curing agent;
s4, adding the fluorescent indicator solution into the matrix solution containing the curing agent according to the ratio of the matrix solution containing the curing agent to the fluorescent indicator solution being 1:10(w/w), stirring to fully mix to obtain a membrane making solution, and putting the membrane making solution into a vacuum pump for vacuumizing to remove air bubbles in the membrane making solution; after the bubbles disappear, introducing the prepared membrane-making solution into a fluorescent membrane reverse mold shown in figures 3-4, and repeatedly exhausting air under a vacuum condition to keep the liquid level; and placing the obtained mould in a heating plate, heating at 65 ℃ for curing for 4h, and then demolding to obtain the fluorescent oxygen sensing film.
(3) Preparation of optical oxygen sensing film
And (3) uniformly coating epoxy resin ultraviolet curing glue on the upper surface of the 3D printing structure of the chip layer, aligning the fluorescent oxygen sensing film prepared in the step (2) to a corresponding part on the 3D printing structure for bonding, and irradiating by using an ultraviolet lamp to cure the fluorescent oxygen sensing film, wherein the curing temperature is 50 ℃, and the curing time is 4 hours, so that the optical oxygen sensing film is obtained.
The structure of the obtained optical oxygen sensing film sheet is shown in figures 1-2, and the material is shown in figure 5.
Example 2: application method of optical oxygen sensing membrane
The performance test of the optical oxygen sensing membrane is carried out by adopting a fluorescence spectrometer, a sample (gas or liquid) to be tested with nitrogen saturation and oxygen saturation is respectively introduced into two channels, the nitrogen and oxygen concentration is adjusted by mixing and adjusting the flow rates of two peristaltic pumps through a three-way valve, the flow rates are connected through a pipeline and finally enter an inlet of the optical oxygen sensing membrane, the optical oxygen sensing membrane is placed in a detection sample pool of the fluorescence spectrometer, the parameters of the spectrometer are adjusted, the excitation wavelength is 460nm, the slit width is 10nm, the collection wavelength range is 480 and 800nm, the fluorescence intensity is detected, and the oxygen concentration is determined.
Fluorescence intensity detection
The optical oxygen sensing film prepared in example 1 was placed in a detection sample cell of a fluorescence spectrometer, and the fluorescence intensity of the fluorescent film was measured using an excitation wavelength of 460nm and a slit width of 10nm, as shown in the figure, fluorescence was observed at 630nm, which corresponds to the emission wavelength of the fluorescent indicator tris (4, 7-biphenyl-1, 10-phenanthroline) ruthenium (ii) complex. It is shown that the fluorescent oxygen sensing film prepared in example 1 can be used for oxygen concentration testing.
Fluorescence lifetime test
The optical oxygen sensing film prepared in example 1 was placed in a sample holder of a fluorescence lifetime tester, and the fluorescence lifetime was measured using an excitation wavelength of 460nm, as shown in fig. 5, to obtain a fluorescence lifetime of 30 ns. It is shown that the fluorescent oxygen sensing film prepared in example 1 can be used for oxygen concentration testing.
The performance of the optical oxygen sensing film is evaluated by performing an oxygen response characteristic test, a response curve, reproducibility, service life, practical application, stability test and the like.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (10)
1. The optical oxygen sensing film piece is characterized by comprising a fluorescent oxygen sensing film layer and a chip layer, wherein the fluorescent oxygen sensing film layer is adhered to the upper surface of the chip layer; two fluid microchannels which are not communicated are arranged in the chip layer, a sample inlet and a sample outlet are arranged at two ends of each fluid microchannel, and two liquid storage tanks are arranged in the middle of each fluid microchannel.
2. The optical oxygen sensing membrane sheet of claim 1, further comprising one or more of the following features:
1) the two unconnected fluid microchannels in the chip layer are arranged in parallel;
2) the liquid storage tank in the chip layer is a cylindrical liquid storage tank;
3) the chip layer is made of transparent photosensitive resin materials.
3. The optical oxygen sensing film sheet of claim 1, wherein the fluorescent oxygen sensing film comprises a polymer matrix and a fluorescent indicator uniformly embedded in the polymer matrix.
4. The optical oxygen sensing membrane sheet of claim 3, further comprising at least one of the following features:
(a) the polymer matrix is selected from one or a combination of polyvinyl alcohol, polyvinyl chloride and polydimethylsiloxane;
(b) the fluorescent indicator is selected from any one of a tris (2, 2' -bipyridyl) ruthenium (II) complex, a tris (1, 10-phenanthroline) ruthenium (II) complex, a tris (4, 7-biphenyl-1, 10-phenanthroline) ruthenium (II) complex or a tris (5-amino-1, 10-phenanthroline) ruthenium (II) complex.
5. A preparation method of an optical oxygen sensing membrane is characterized by comprising the following steps:
step one, 3D printing a three-dimensional model of a chip layer to obtain a printing structure, and carrying out ultraviolet curing on the printing structure to obtain the chip layer;
step two, preparing a fluorescent oxygen sensing film layer;
and step three, uniformly coating an ultraviolet curing adhesive on the upper surface of the chip layer, correspondingly adhering the fluorescent oxygen sensing film layer and the upper surface of the chip layer, and curing under ultraviolet light to obtain the optical oxygen sensing film.
6. The method of making an optical oxygen sensing membrane sheet of claim 5, further comprising one or more of the following features:
1) in the first step, software adopted by the 3D printer is Preform;
2) setting a chip layer supporting structure, a layering thickness, printing material attributes and proportioning parameters before printing;
3) in the first step, the printing structure needs to be soaked in cleaning liquid for 2-4 hours before ultraviolet curing;
4) in the first step, the ultraviolet curing temperature is 35-80 ℃, and the curing time is 3-10 h;
5) the structure of the fluorescent film layer in the third step is completely matched with the printing structure of the chip layer in the first step;
6) the ultraviolet curing adhesive in the third step is an epoxy resin adhesive;
7) in the third step, the ultraviolet curing temperature is 35-80 ℃, and the curing time is 3-5 hours.
7. The method of manufacturing an optical oxygen sensing membrane sheet according to claim 5, wherein the step two of manufacturing the fluorescent oxygen sensing membrane layer specifically comprises the following operations:
s1, preparing a fluorescent indicator solution;
s2, preparing a polymer matrix solution;
s3, uniformly mixing the polymer matrix solution with a curing agent to obtain a matrix solution containing the curing agent;
and S4, adding the fluorescent indicator solution into the matrix solution containing the curing agent according to the weight ratio, uniformly mixing to obtain a membrane making solution, removing bubbles in the membrane making solution, introducing the membrane making solution into a reverse mold, heating for curing, and demolding to obtain the fluorescent oxygen sensing membrane layer.
8. The method of making an optical oxygen sensing membrane sheet of claim 7, further comprising one or more of the following features:
(1) the weight ratio of the fluorescent indicator to the organic solvent in the fluorescent indicator solution in S1 is 1: 8-10;
(2) the weight ratio of the curing agent to the polymer matrix solution in S3 is 1: 8-10;
(3) the weight ratio of the fluorescent indicator solution to the matrix solution containing the curing agent in S4 is 1: 8-10;
(4) the specific operation of removing the bubbles in the membrane-making solution in the S4 is to put the membrane-making solution into a vacuum pump for vacuumizing;
(5) repeatedly exhausting air in vacuum before heating and curing in the S4 to keep the liquid level;
(6) in S4, the heating curing temperature is 55-90 ℃, and the curing time is 3-8 h.
9. The method for producing an optical oxygen sensing membrane sheet according to claim 8, wherein the organic solvent in the step (1) is selected from any one of ethanol, toluene, dichloromethane, chloroform, and N, N-dimethylformamide.
10. Use of the optical oxygen sensing film sheet according to any one of claims 1 to 4 or the optical oxygen sensing film sheet prepared by the method according to any one of claims 5 to 9 for oxygen sensing detection.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210011315.0A CN114324285A (en) | 2022-01-06 | 2022-01-06 | Optical oxygen sensing membrane and preparation method and application thereof |
| CN202211665673.XA CN115931726A (en) | 2022-01-06 | 2022-12-23 | Optical oxygen sensing membrane and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210011315.0A CN114324285A (en) | 2022-01-06 | 2022-01-06 | Optical oxygen sensing membrane and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114324285A true CN114324285A (en) | 2022-04-12 |
Family
ID=81024150
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210011315.0A Pending CN114324285A (en) | 2022-01-06 | 2022-01-06 | Optical oxygen sensing membrane and preparation method and application thereof |
| CN202211665673.XA Pending CN115931726A (en) | 2022-01-06 | 2022-12-23 | Optical oxygen sensing membrane and preparation method and application thereof |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211665673.XA Pending CN115931726A (en) | 2022-01-06 | 2022-12-23 | Optical oxygen sensing membrane and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN114324285A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115595141A (en) * | 2022-09-30 | 2023-01-13 | 浙江清华柔性电子技术研究院（Cn） | Method for manufacturing oxygen sensor fluorescent film, oxygen sensor fluorescent film and oxygen sensor |
-
2022
- 2022-01-06 CN CN202210011315.0A patent/CN114324285A/en active Pending
- 2022-12-23 CN CN202211665673.XA patent/CN115931726A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115595141A (en) * | 2022-09-30 | 2023-01-13 | 浙江清华柔性电子技术研究院（Cn） | Method for manufacturing oxygen sensor fluorescent film, oxygen sensor fluorescent film and oxygen sensor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115931726A (en) | 2023-04-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Li et al. | Optical characteristics of a ruthenium (II) complex immobilized in a silicone rubber film for oxygen measurement | |
| Vollmer et al. | Development of an integrated microfluidic platform for dynamic oxygen sensing and delivery in a flowing medium | |
| Lobnik et al. | Optical chemical sensors: design and applications | |
| EP2635624B1 (en) | Optical sensor and sensing system for oxygen monitoring in fluids using molybdenum cluster phosphorescence | |
| Mao et al. | Honeycomb structured porous films from a platinum porphyrin-grafted poly (styrene-co-4-vinylpyridine) copolymer as an optical oxygen sensor | |
| CN115931726A (en) | Optical oxygen sensing membrane and preparation method and application thereof | |
| CN104865292B (en) | A kind of nitrogen dioxide gas sensor based on o-aminophenyl substitution porphyrin nano material | |
| CN104650374B (en) | A kind of preparation method of metalloporphyrin the oxygen sensing film | |
| CN108003374B (en) | Molecular imprinting photonic crystal hydrogel film for rapidly detecting melamine | |
| CN110907445A (en) | Microfluidic biochip detection device, preparation method and detection method | |
| CN110108683B (en) | Preparation method of ratio oxygen sensing film for dissolved oxygen content detection | |
| Toda et al. | Micro-gas analysis system μGAS comprising a microchannel scrubber and a micro-fluorescence detector for measurement of hydrogen sulfide | |
| Lu et al. | An online pH detection system based on a microfluidic chip | |
| CN108896539A (en) | Measure the optofluidic detector of phosphorus content in seawater | |
| CN114088697B (en) | Microfluidic chip device for biogenic amine detection and application | |
| Fujii et al. | Fluorometric determination of sulfite and nitrite in aqueous samples using a novel detection unit of a microfluidic device | |
| Holobar et al. | Experimental results on an optical pH measurement system for bioreactors | |
| KR102056219B1 (en) | pH DETECTING MICRO-STRUCTURED STICKER AND THE MANUFACTURING METHOD THEREOF | |
| CN110554015B (en) | Method for realizing visual detection of Cr (VI) by micro-fluidic sensor based on photoluminescence xylan carbon quantum dots | |
| CN106855513A (en) | A kind of assay method of oxygen in water | |
| CN108514899A (en) | A kind of paper substrate micro-fluidic chip system quickly detected for pollutant trace metal | |
| Kenley et al. | Photooxidation of di-n-butyl sulfide using sensitizers immobilized in polymer films | |
| CN107677657B (en) | Fluorescence detection pool for detecting concentration of dissolved oxygen and manufacturing method thereof | |
| JP2014142220A (en) | pH MEASURING SYSTEM, pH MEASURING DEVICE, AND pH SENSING SHEET AND MANUFACTURING METHOD THEREOF | |
| Mohr | Polymers for optical sensors |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20220412 |
|
| WD01 | Invention patent application deemed withdrawn after publication |