Method and device for measuring proportional oxygen concentration of wood-based composite oxygen sensing material

Abstract

The invention discloses a method and a device for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material, and relates to the field of oxygen measurement. The technical problems that how to utilize wood to be compounded with metalloporphyrin, overcome the influence of excitation light source power on a test result and improve the anti-interference capability and stability of a sensor and the oxygen concentration test range in the prior art are solved. According to the invention, balsa wood is taken as a wood-based material, and metalloporphyrin Gd-HMME is embedded into the balsa wood, so that under the excitation of an ultraviolet laser, the ratio of a fluorescence signal to a phosphorescence signal of the wood-based composite material is taken as an optical parameter, and the oxygen concentration test is realized. The method is also suitable for the field of sensor preparation.

Description

Technical Field

[0001] The present invention relates to the technical field of oxygen measurement, and particularly relates to a method and device for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material. Background Art

[0002] Oxygen is one of the most important chemical elements on Earth. It exists widely in nature and plays a crucial role in various fields. Accurately measuring the oxygen concentration is of great significance in many fields such as scientific research, industrial production, and environmental monitoring. For example, in battery development, changes in oxygen concentration can significantly affect the performance of the battery. Too high or too low oxygen concentration may lead to a decline in battery performance, or even shorten the cycle life or pose a threat to safety. In the process of steel smelting, the oxygen concentration directly affects the combustion efficiency in the furnace and the quality of molten iron. Fluctuations in oxygen concentration will increase the instability of the chemical composition and alloy properties of steel. In semiconductor manufacturing, the oxygen concentration is crucial for controlling thin film growth, the quality of the oxide layer, and the doping process. Thus, it can be seen that the precise regulation of oxygen concentration has a direct and crucial impact on ensuring product quality, improving production efficiency, and guaranteeing safety. Therefore, the detection of oxygen concentration has become a core technical requirement in various fields.

[0003] Currently, the detection methods of oxygen concentration mainly include electrochemistry sensing method, iodometry, optical sensing method (such as phosphorescence measurement technology), etc. Among them, due to its advantages such as non-contact, high sensitivity, and rapid response, phosphorescence measurement technology has been widely used in oxygen concentration measurement. However, there are still some deficiencies in the existing phosphorescence-based oxygen sensing methods. Phosphorescence oxygen sensing technology relies on the change of the luminescence signal of oxygen-sensitive molecules, and the test results are easily affected by the power of the excitation light source, resulting in poor test stability. In addition, existing phosphorescence oxygen sensors mostly use traditional oxygen-sensitive molecules, and these oxygen-sensitive molecules may be affected by interfering gases under certain environmental conditions, thereby reducing the accuracy and reliability of the sensor. Another problem is that existing oxygen sensor materials are mostly high-cost or non-renewable materials, which are difficult to meet the requirements of environmentally friendly and low-cost applications.

[0004] To solve these problems, some new oxygen sensor technologies have emerged in recent years, and the research on wood as a support material has received attention. As a natural, environmentally friendly, and renewable material, wood has the advantages of stable structure, strong mechanical properties, and loose porosity, etc., which can effectively support the attachment of oxygen-sensitive molecules and promote the diffusion of oxygen.

[0005] However, most of the existing wood-based oxygen sensors focus on material preparation and performance optimization, and still lack the full utilization of proportional oxygen measurement technology and the effective suppression of the interference of the excitation light source. Therefore, how to use wood and metal porphyrin composites to overcome the influence of the excitation light source power on the test results and improve the sensor's anti-interference ability and stability as well as the oxygen concentration test range has become a technical problem that needs to be solved urgently. Summary of the invention

[0006] The present invention aims to solve the existing technical problems of how to utilize wood and metal porphyrin to compound, overcome the influence of the excitation light source power on the test results, and improve the anti-interference ability and stability of the sensor as well as the oxygen concentration test range, which have become technical problems to be solved urgently.

[0007] To solve the above technical problems, the present invention is achieved through the following technical solutions:

[0008] Solution 1: The present invention proposes a method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensor material, the method comprising the following steps:

[0009] Step 1, placing balsa wood slices in an organic solvent containing metal porphyrin Gd-HMME for full immersion, taking them out and drying them to obtain a composite material of balsa wood and metal porphyrin Gd-HMME, and moving the composite material of balsa wood and metal porphyrin Gd-HMME into a gas chamber;

[0010] Step 2: introducing nitrogen in a nitrogen cylinder and oxygen in an oxygen cylinder into a gas mixing chamber at different flow rates through a first mass flow meter and a second mass flow meter, respectively, to prepare oxygen of different concentrations; introducing oxygen of different concentrations into the gas chamber described in step 1;

[0011] Step 3, using an ultraviolet laser as an incident light source to irradiate the gas chamber, and measuring the photoluminescence spectrum of the balsa wood and metalloporphyrin Gd-HMME composite material under different oxygen concentrations by using a spectrometer;

[0012] Step 4, integrating the fluorescence signal and the phosphorescence signal in the photoluminescence spectrum in step 3 respectively, and obtaining S1=k1I, S2=k2Ih(C0); wherein S1 is the integral of the fluorescence signal, S2 is the integral of the phosphorescence signal, k1 and k2 are both constants, I is the intensity of the ultraviolet laser light source, C0 is the oxygen concentration, and h(C0) is the oxygen concentration relationship;

[0013] Step 5: Perform ratio processing on the integral of the fluorescence signal and the phosphorescence signal in step 4 to obtain the relationship between the optical parameter OP and the oxygen concentration, that is, The optical parameter OP is expressed as the ratio of the integral results of the fluorescence signal and the phosphorescence signal, and k is a constant.

[0014] Further, a preferred embodiment is provided, wherein the organic solvent described in step 1 is methanol.

[0015] Further, a preferred embodiment is provided, wherein the time for fully impregnating the balsa wood slices in the organic solvent containing metal porphyrin Gd-HMME is 20 min to 120 min.

[0016] Further, a preferred embodiment is provided, wherein the total flow rate of nitrogen in the nitrogen gas cylinder and oxygen in the oxygen gas cylinder described in step 2 is 2 L / min.

[0017] Further, a preferred embodiment is provided, wherein the emission wavelength of the ultraviolet laser described in step 3 is 405 nm.

[0018] Further, a preferred embodiment is provided, wherein the relationship between the optical parameter OP and the oxygen concentration obtained by ratio processing of the integrals of the fluorescence signal and phosphorescence signal in step 4 in step 5 includes:

[0019] First, a linear equation OP = aC0 + b is obtained by linear fitting of the ratio of the known concentration of oxygen and the integral result. After calculating the ratio of the integral results of the actually measured fluorescence signal and phosphorescence signal, the oxygen concentration value to be measured is obtained through this linear equation; where a and b both represent linear coefficients.

[0020] Further, a preferred embodiment is provided, wherein in step 5, the ratio processing of the integrals of the fluorescence signal and phosphorescence signal in step 4 uses the spectral information in the wavelength range of 480 nm to 520 nm of the emission spectrum as the fluorescence signal, and the spectral information in the wavelength range of 712 nm to 790 nm as the phosphorescence signal.

[0021] Solution 2: A proportional oxygen concentration measuring device for a wood-based composite oxygen sensing material, the device is implemented based on the method described in Solution 1, and the device includes:

[0022] A wood-based composite oxygen sensing material preparation module, configured to fully impregnate balsa wood slices in an organic solvent containing metal porphyrin Gd-HMME, take them out and dry them to obtain a balsa wood and metal porphyrin Gd-HMME composite material, and transfer the balsa wood and metal porphyrin Gd-HMME composite material into a gas chamber;

[0023] An oxygen preparation module, configured to respectively pass nitrogen in a nitrogen gas cylinder and oxygen in an oxygen gas cylinder into a mixing chamber at different flow rates through a first mass flowmeter and a second mass flowmeter to prepare oxygen with different concentrations; and pass the oxygen with different concentrations into the gas chamber of the wood-based composite oxygen sensing material preparation module;

[0024] A photoluminescence spectrum determination module, which is used to irradiate a gas chamber with an ultraviolet laser as an incident light source, and measure the photoluminescence spectra of the balsa and the metal porphyrin Gd-HMME composite material at different oxygen concentrations through a spectrometer;

[0025] A signal integration module, which is used to integrate the fluorescence signal and the phosphorescence signal in the photoluminescence spectrum in the photoluminescence spectrum determination module respectively, that is, S1 = k1I, S2 = k2Ih(C0); where S1 is the integration of the fluorescence signal, S2 is the integration of the phosphorescence signal, both k1 and k2 are constants, I is the intensity of the ultraviolet laser light source, C0 is the oxygen concentration, and h(C0) is the oxygen concentration relationship formula;

[0026] An oxygen concentration value determination module, which is used to process the ratio of the integration of the fluorescence signal and the phosphorescence signal in the signal integration module to obtain the relationship between the optical parameter OP and the oxygen concentration, that is where the optical parameter OP is expressed as the ratio of the integration results of the fluorescence signal and the phosphorescence signal, and k is a constant.

[0027] Solution Three: A computer device, including a memory and a processor, where a computer program is stored in the memory. When the processor runs the computer program stored in the memory, the processor executes the method described in any one of Solution One.

[0028] Solution Four: A computer-readable storage medium, where a computer program is stored in the computer-readable storage medium. When the computer program is executed by a processor, the steps of the method described in any one of Solution One are implemented.

[0029] The beneficial effects of the present invention are as follows:

[0030] For the method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material described in the present invention, through experiments, it is verified that the present invention loads the metal porphyrin Gd-HMME on the balsa wood slices, can realize the measurement of the oxygen concentration, and significantly reduces the influence brought by the laser power fluctuation. When the laser power is less than 3.6 mW / cm 2 the change of the laser power will not affect the test result of the oxygen concentration.

[0031] The method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material described in the present invention can realize the high-precision measurement of the oxygen concentration. By using the integration ratio of the fluorescence signal and the phosphorescence signal of the photoluminescence spectrum of the wood-based composite material at different oxygen concentrations, an accurate calibration curve or equation can be established, so as to realize the precise measurement with the relative uncertainty of the oxygen concentration test result less than 1.4%.

[0032] The method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material described in the present invention has a strong anti-laser power interference ability, theoretically eliminating the influence of laser power fluctuations on the measurement of oxygen concentration. Through experimental verification, when the laser power is less than 3.6 mW / cm 2 no influence is produced on the measurement of oxygen concentration due to the fluctuations brought by the laser power.

[0033] In the method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material described in the present invention, the method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material can cover a relatively wide oxygen concentration range and can achieve the measurement of oxygen concentration from 0 to 100 kPa.

[0034] The method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material described in the present invention can have a relatively fast response speed to oxygen, with a fast response time of up to 3.6 s. This is very important for applications that require real-time detection and regulation of oxygen concentration.

[0035] In the present invention, the wood-based composite oxygen sensing material uses natural balsa wood as the support material, which has the advantages of being green, environmentally friendly, and degradable.

[0036] The present invention is also applicable to the field of sensor preparation. Brief Description of the Drawings

[0037] Figure 1 It is a schematic flow chart of the method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material described in Embodiment 1.

[0038] Figure 2 It is a schematic flow chart of the device for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material described in Embodiment 8.

[0039] Figure 3 It is a schematic diagram of the changes in the absorption spectrum and photoluminescence spectrum of Gd-HMME in methanol solution described in Embodiment 11.

[0040] Figure 4 It is a photoluminescence spectrum of balsa wood and a luminescence spectrum diagram of the wood-based composite oxygen sensing material in pure nitrogen and pure oxygen described in Embodiment 11.

[0041] Figure 5 It is a schematic diagram of the integration regions of the fluorescence signal S1 and phosphorescence signal S2 of the wood-based composite oxygen sensing material described in Embodiment 11.

[0042] Figure 6 It is the photoluminescence spectrum of the wood-based composite oxygen sensing material under different oxygen concentrations described in Embodiment 11.

[0043] Figure 7Graph showing the relationship between the optical parameter OP of the wood-based composite oxygen sensing material described in Embodiment XI and the oxygen concentration.

[0044] Figure 8 Graph showing the relationship between the fluorescence signal integral S1, the phosphorescence signal integral S2, and the optical parameter OP of the wood-based composite oxygen sensing material described in Embodiment XI under different laser powers.

[0045] Figure 9 Graph showing 100 sets of S1, S2, and OP data points collected statically for the wood-based composite oxygen sensing material described in Embodiment XI.

[0046] Figure 10 Graph showing the test results of the response time and recovery time of the wood-based composite oxygen sensing material described in Embodiment XI.

[0047] Among them, nitrogen gas cylinder 1, first mass flowmeter 2, second mass flowmeter 3, oxygen gas cylinder 4, mixing chamber 5, ultraviolet laser 6, gas chamber 7, spectrometer 8, computer 9. Specific embodiments

[0048] To make the objectives, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, rather than all of the embodiments.

[0049] Embodiment 1. This embodiment proposes a method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material, and the method includes the following steps:

[0050] Step 1. Immerse balsa wood slices in an organic solvent containing metal porphyrin Gd-HMME, take them out and dry to obtain a balsa wood and metal porphyrin Gd-HMME composite material, and transfer the balsa wood and metal porphyrin Gd-HMME composite material into the gas chamber 7;

[0051] Step 2. Pass nitrogen from the nitrogen gas cylinder 1 and oxygen from the oxygen gas cylinder 4 into the mixing chamber 5 at different flow rates through the first mass flowmeter 2 and the second mass flowmeter 3 respectively to prepare oxygen with different concentrations; pass the oxygen with different concentrations into the gas chamber 7 described in Step 1;

[0052] Step 3. Use the ultraviolet laser 6 as the incident light source to irradiate the gas chamber 7, and measure the photoluminescence spectrum of the balsa wood and metal porphyrin Gd-HMME composite material at different oxygen concentrations through the spectrometer 8;

[0053] Step 4: Integrate the fluorescence signal and phosphorescence signal in the photoluminescence spectrum in Step 3, i.e., S1 = k1I, S2 = k2Ih(C0); where S1 is the integration of the fluorescence signal, S2 is the integration of the phosphorescence signal, k1 and k2 are both constants, I is the intensity of the ultraviolet laser light source, C0 is the oxygen concentration, and h(C0) is the oxygen concentration relationship formula.

[0054] Step 5: Process the integration of the fluorescence signal and phosphorescence signal in Step 4 by taking the ratio to obtain the relationship between the optical parameter OP and the oxygen concentration, i.e., where the optical parameter OP is expressed as the ratio of the integration results of the fluorescence signal and phosphorescence signal, and k is a constant.

[0055] Embodiment 2: This embodiment further limits the proportional oxygen concentration measurement method of a wood-based composite oxygen sensing material described in Embodiment 1. The organic solvent described in Step 1 is methanol.

[0056] Embodiment 3: This embodiment further limits the proportional oxygen concentration measurement method of a wood-based composite oxygen sensing material described in Embodiment 1. The time for fully impregnating the balsa wood slices in the organic solvent containing metal porphyrin Gd-HMME is 20 min to 120 min.

[0057] Embodiment 4: This embodiment further limits the proportional oxygen concentration measurement method of a wood-based composite oxygen sensing material described in Embodiment 1. The total flow rate of the nitrogen in the nitrogen gas cylinder 1 and the oxygen in the oxygen gas cylinder 4 in Step 2 is 2 L / min.

[0058] Embodiment 5: This embodiment further limits the proportional oxygen concentration measurement method of a wood-based composite oxygen sensing material described in Embodiment 1. The emission wavelength of the ultraviolet laser 6 in Step 3 is 405 nm.

[0059] Embodiment 6: This embodiment further limits the proportional oxygen concentration measurement method of a wood-based composite oxygen sensing material described in Embodiment 1. The relationship between the optical parameter OP and the oxygen concentration obtained by processing the integration of the fluorescence signal and phosphorescence signal in Step 4 by taking the ratio includes:

[0060] First, perform linear fitting on the ratio of the known concentration of oxygen and the integration result to obtain a linear equation OP = aC0 + b. After calculating the ratio of the integration results obtained from the actually measured fluorescence signal and phosphorescence signal, obtain the value of the oxygen concentration to be measured through this linear equation; where a and b both represent linear coefficients.

[0061] Embodiment 7. This embodiment further limits the method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material described in Embodiment 1. In step 5, when performing ratio processing on the integrals of the fluorescence signal and phosphorescence signal in step 4, the spectral information in the wavelength range of 480 nm to 520 nm of the emission spectrum is used as the fluorescence signal, and the spectral information in the wavelength range of 712 nm to 790 nm is used as the phosphorescence signal.

[0062] Embodiment 8. This embodiment proposes a device for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material. The device is implemented based on the method described in Embodiment 1, and the device includes:

[0063] A wood-based composite oxygen sensing material preparation module, which is used to fully immerse balsa wood slices in an organic solvent containing metal porphyrin Gd-HMME, take them out and dry them to obtain a balsa wood and metal porphyrin Gd-HMME composite material, and transfer the balsa wood and metal porphyrin Gd-HMME composite material into the gas chamber 7;

[0064] An oxygen preparation module, which is used to introduce nitrogen in the nitrogen gas cylinder 1 and oxygen in the oxygen gas cylinder 4 into the mixing chamber 5 at different flow rates through the first mass flowmeter 2 and the second mass flowmeter 3 respectively to prepare oxygen with different concentrations; and introduce the oxygen with different concentrations into the gas chamber 7 of the wood-based composite oxygen sensing material preparation module;

[0065] A photoluminescence spectrum determination module, which is used to irradiate the gas chamber 7 with an ultraviolet laser 6 as the incident light source, and measure the photoluminescence spectra of the balsa wood and metal porphyrin Gd-HMME composite material at different oxygen concentrations through a spectrometer 8;

[0066] A signal integration module, which is used to integrate the fluorescence signal and phosphorescence signal in the photoluminescence spectrum in the photoluminescence spectrum determination module respectively, that is, S1 = k1I, S2 = k2Ih(C0); where S1 is the integral of the fluorescence signal, S2 is the integral of the phosphorescence signal, k1 and k2 are both constants, I is the intensity of the ultraviolet laser light source, C0 is the oxygen concentration, and h(C0) is the oxygen concentration relationship;

[0067] An oxygen concentration value determination module, which is used to perform ratio processing on the integrals of the fluorescence signal and phosphorescence signal in the signal integration module to obtain the relationship between the optical parameter OP and the oxygen concentration, that is where the optical parameter OP is expressed as the ratio of the integral results of the fluorescence signal and phosphorescence signal, and k is a constant.

[0068] Embodiment 9. This embodiment proposes a computer device, including a memory and a processor. A computer program is stored in the memory. When the processor runs the computer program stored in the memory, the processor executes the method described in any one of Embodiments 1 to 7.

[0069] Embodiment 10. This embodiment proposes a computer-readable storage medium. The computer-readable storage medium stores a computer program. When the computer program is executed by a processor, the steps of the method described in any one of Embodiments 1 to 7 are implemented.

[0070] Embodiment 11. This embodiment proposes an example, and the example is used to explain the above Embodiments 1 to 10. The example is specifically as follows:

[0071] See Figures 1 to 10 To illustrate this embodiment, this embodiment specifically includes the following steps:

[0072] The purpose of the present invention is to provide a method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material. The present invention uses balsa wood as the wood-based material. By embedding metal porphyrin Gd-HMME into the balsa wood, it is found that under the excitation of an ultraviolet laser, using the ratio of the fluorescence signal to the phosphorescence signal of the wood-based composite material as an optical parameter can realize the measurement of oxygen concentration.

[0073] The present invention uses balsa wood as the wood-based material. By embedding metal porphyrin Gd-HMME into the balsa wood, it is found that under the excitation of an ultraviolet laser, using the ratio of the fluorescence signal to the phosphorescence signal of the wood-based composite material as an optical parameter can theoretically eliminate the influence brought by the fluctuation of the laser power, making the measurement of oxygen concentration more accurate.

[0074] Specifically, as Figure 1 shown is the method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material proposed in the embodiment of the present invention. The method includes the following steps:

[0075] Step 1. Place the balsa wood slices in an organic solvent of Gd-HMME for sufficient impregnation. After taking them out and drying, obtain the balsa wood and Gd-HMME composite material, and then move the balsa wood and Gd-HMME composite material into a gas chamber.

[0076] In this embodiment, the size of the balsa wood slices is 2 cm × 2 cm × 0.8 cm (longitudinal × tangential × radial).

[0077] In this embodiment, for the sufficient impregnation, the time is 20 min to 120 min.

[0078] See Figure 2As shown, in Step 2, nitrogen and oxygen are introduced into the gas mixing chamber 5 at different flow rates through the first mass flowmeter 2 and the second mass flowmeter 3 respectively to prepare oxygen with different concentrations. The oxygen with different concentrations is introduced into the gas chamber 7.

[0079] In this embodiment, the total gas flow rate of nitrogen and oxygen remains unchanged. The total gas flow rate is preferably 2 L / min.

[0080] In Step 3, an ultraviolet laser is used as the incident light source to irradiate the gas chamber, and the photoluminescence spectra of balsa wood and Gd-HMME composite material at different oxygen concentrations are measured by a spectrometer.

[0081] See Figure 3 as shown, Figure 3 The chemical structural formula of Gd-HMME is shown. The light source of the absorption spectrum is a deuterium lamp, and the excitation light source of the emission spectrum is a 405 nm laser. In this embodiment, the ultraviolet laser 6 is a continuous semiconductor laser, and preferably a 405 nm continuous semiconductor laser.

[0082] In Step 4, the fluorescence signal and the phosphorescence signal in the photoluminescence spectrum obtained in Step 3 are integrated respectively. The integration of the fluorescence signal is only related to the intensity of the incident light source, while the integration of the phosphorescence signal is related to both the intensity of the incident light source and the oxygen concentration. That is, S1 = k1I, S2 = k2Ih(C0). Where S1 is the integration of the fluorescence signal, S2 is the integration of the phosphorescence signal, k1 and k2 are both constants, I is the intensity of the ultraviolet laser light source in Step 3, C0 is the oxygen concentration, and h(C0) is the oxygen concentration relationship formula.

[0083] See Figure 4 as shown, Figure 4 The emission spectra of balsa wood and the emission spectra of the wood-based composite oxygen sensing material in pure nitrogen and pure oxygen are shown. The excitation light source of the emission spectrum is a 405 nm laser. In this embodiment, the fluorescence signal is preferably the spectral signal of the photoluminescence spectrum in the range of 480 nm to 520 nm in Step 3; the phosphorescence signal is preferably the spectral signal of the photoluminescence spectrum in the range of 712 nm to 790 nm in Step 3.

[0084] In Step 5, the integration of the fluorescence signal and the phosphorescence signal in Step 4 is ratio-processed, that is, the relationship between the optical parameter OP and the oxygen concentration is obtained, that is where the optical parameter OP is expressed as the ratio of the integration results of the fluorescence signal and the phosphorescence signal, and k is a constant. The expression of OP has nothing to do with the excitation light power I. Therefore, the method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material theoretically eliminates the influence brought by the fluctuation of the excitation light power.

[0085] See Figure 5 as shown Figure 5 It is a schematic diagram of the integration regions of the fluorescence signal S1 and the phosphorescence signal S2 of the wood-based composite oxygen sensing material. The integration region of S1 is 480 nm to 520 nm, and the integration region of S2 is 712 nm to 790 nm. Figure 6 It is the emission spectrum of the wood-based composite oxygen sensing material under different oxygen concentrations. The excitation light source of the emission spectrum is a 405 nm laser.

[0086] Step six, the oxygen concentration values obtained from the ratio of the integration results in Step four include: first, a linear equation OP = aC0 + b is obtained by linear fitting of the ratio of the known concentration of oxygen and the integration result, and then the ratio of the integration results calculated from the actually measured fluorescence signal and phosphorescence signal is used to obtain the oxygen concentration value to be measured through this linear equation; where a and b both represent linear coefficients.

[0087] Figure 7 It is a relationship diagram between the optical parameter OP of the wood-based composite oxygen sensing material and the oxygen concentration. Figure 8 It is a relationship diagram between the fluorescence signal integration S1, the phosphorescence signal integration S2, and the optical parameter OP under different laser powers. Figure 9 It is a diagram of 100 groups of S1, S2, and OP data points collected statically. The light source used is a 405 nm laser with a power of 0.12 mW / cm 2 . Figure 10 It is a test result diagram of the response time and recovery time of the wood-based composite oxygen sensing material. The response time is 3.6 s, and the recovery time is 4.9 s.

[0088] In summary, the present invention establishes a method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material. Through experimental verification, the present invention loads Gd-HMME on balsa wood slices, can achieve the measurement of oxygen concentration, significantly reduce the influence brought by laser power fluctuations. When the laser power is less than 3.6 mW / cm 2 , the change in laser power will not affect the test result of oxygen concentration.

[0089] Those skilled in the art can understand that the above is only the preferred embodiment of the present invention. The features recorded in each embodiment and / or claim of the present disclosure can be combined or combined in various ways, even if such combinations or combinations are not explicitly recorded in the present disclosure. It is not used to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some of the technical features. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

[0090] Although the preferred embodiments of the present invention have been described, additional changes and modifications can be made by those skilled in the art once they learn the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications that fall within the scope of the present invention. Obviously, those skilled in the art can make various changes and variations to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalent technologies, the present invention is also intended to include these modifications and variations.

Claims

1. A method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material, characterized in that: The method comprises the following steps: Step 1, placing balsa wood slices in an organic solvent containing metal porphyrin Gd-HMME for full immersion, taking out and drying to obtain a balsa wood and metal porphyrin Gd-HMME composite material, and moving the balsa wood and metal porphyrin Gd-HMME composite material into a gas chamber (7); Step 2: introducing nitrogen in the nitrogen cylinder (1) and oxygen in the oxygen cylinder (4) into the gas mixing chamber (5) at different flow rates through the first mass flow meter (2) and the second mass flow meter (3) respectively, to prepare oxygen with different concentrations; introducing oxygen with different concentrations into the gas chamber (7) described in step 1; Step 3, using an ultraviolet laser (6) as an incident light source to illuminate the gas chamber (7), and measuring the photoluminescence spectrum of the balsa wood and metalloporphyrin Gd-HMME composite material under different oxygen concentrations using a spectrometer (8); Step 4, integrating the fluorescence signal and the phosphorescence signal in the photoluminescence spectrum in step 3, that is, S1=k1I, S2=k2Ih(C0); wherein S1 is the integral of the fluorescence signal, S2 is the integral of the phosphorescence signal, k1 and k2 are both constants, I is the intensity of the ultraviolet laser light source, C0 is the oxygen concentration, and h(C0) is the oxygen concentration relationship; Step 5: Perform ratio processing on the integral of the fluorescence signal and the phosphorescence signal in step 4 to obtain the relationship between the optical parameter OP and the oxygen concentration, that is, The optical parameter OP is expressed as the ratio of the integral results of the fluorescence signal and the phosphorescence signal, and k is a constant.

2. The method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material according to claim 1, characterized in that: The organic solvent described in step 1 is methanol.

3. The method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material according to claim 1, characterized in that: The balsa wood slices are placed in an organic solvent containing the metalloporphyrin Gd-HMME and are fully immersed for 20 minutes to 120 minutes.

4. The method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material according to claim 1, characterized in that: The total flow rate of the nitrogen in the nitrogen cylinder (1) and the oxygen in the oxygen cylinder (4) in step 2 is 2 L / min.

5. The method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material according to claim 1, characterized in that: The emission wavelength of the ultraviolet laser (6) described in step 3 is 405 nm.

6. The method for measuring the proportional oxygen concentration of the wood-based composite oxygen sensing material according to claim 1, characterized in that: In step 5, by performing ratio processing on the integral of the fluorescence signal and the phosphorescence signal in step 4, the relationship between the optical parameter OP and the oxygen concentration is obtained, including: First, a linear fitting is performed through the ratio of the known concentration of oxygen and the integral result to obtain the linear equation OP=aC0+b, and the ratio of the integral results obtained by calculating the actual measured fluorescence signal and phosphorescence signal is used to obtain the measured oxygen concentration value through the linear equation; wherein a and b both represent linear coefficients.

7. The method for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material according to claim 1, characterized in that: In step 5, the integral of the fluorescence signal and the phosphorescence signal in step 4 is ratio-processed, and the spectral information of the luminescence spectrum in the 480nm-520nm band is used as the fluorescence signal, and the spectral information in the 712nm-790nm band is used as the phosphorescence signal.

8. A device for measuring the proportional oxygen concentration of a wood-based composite oxygen sensing material, characterized in that: The device is implemented based on the method according to claim 1, and the device comprises: A wood-based composite oxygen sensing material preparation module is used to place balsa wood slices in an organic solvent containing metal porphyrin Gd-HMME for full immersion, take them out and dry them to obtain a balsa wood and metal porphyrin Gd-HMME composite material, and move the balsa wood and metal porphyrin Gd-HMME composite material into a gas chamber (7); The oxygen preparation module is used to pass the nitrogen in the nitrogen cylinder (1) and the oxygen in the oxygen cylinder (4) into the gas mixing chamber (5) at different flow rates through the first mass flow meter (2) and the second mass flow meter (3) to prepare oxygen with different concentrations; and pass the oxygen with different concentrations into the gas chamber (7) described in the wood-based composite oxygen sensor material preparation module; A photoluminescence spectrum determination module is used to use an ultraviolet laser (6) as an incident light source to irradiate a gas chamber (7), and to measure the photoluminescence spectrum of the balsa wood and metalloporphyrin Gd-HMME composite material under different oxygen concentrations through a spectrometer (8); A signal integration module is used to integrate the fluorescence signal and the phosphorescence signal in the photoluminescence spectrum in the photoluminescence spectrum determination module, that is, S1=k1I, S2=k2Ih(C0); wherein S1 is the integral of the fluorescence signal, S2 is the integral of the phosphorescence signal, k1 and k2 are both constants, I is the intensity of the ultraviolet laser light source, C0 is the oxygen concentration, and h(C0) is the oxygen concentration relationship; The oxygen concentration value determination module is used to perform ratio processing on the integral of the fluorescence signal and the phosphorescence signal in the signal integration module to obtain the relationship between the optical parameter OP and the oxygen concentration, that is, The optical parameter OP is expressed as the ratio of the integral results of the fluorescence signal and the phosphorescence signal, and k is a constant.

9. A computer device comprising a memory and a processor, characterized in that A computer program is stored in the memory. When the processor runs the computer program stored in the memory, the processor executes the method according to any one of claims 1 to 7.

10. A computer-readable storage medium, characterized in that The computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the steps of the method according to any one of claims 1 to 7 are implemented.

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