Optical fiber temperature sensor prepared from Eu < 2 + > ion doped zeolite
Eu2+ ion doped zeolite material is prepared by high-temperature reduction method, coated on the end of the optical fiber to form a high-sensitivity fiber temperature sensor, which solves the measurement accuracy and safety problems of traditional sensors in strong electromagnetic and flammable and explosive environments, and achieves higher sensitivity and stability.
Patent Information
- Application Number
- CN202510670181.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-04
- Publication Date
- 2025-08-15
AI Technical Summary
Traditional temperature sensors have reduced or damaged measurement accuracy in strong electromagnetic environments, and have safety hazards in flammable and explosive environments. The sensitivity of existing fiber optic temperature sensors with rare earth ion doped fluorescent materials is insufficient.
The Eu2+ ion-doped zeolite material was prepared by high-temperature reduction method. By composite coating with resin on the end of the optical fiber, an optical fiber temperature sensor prepared by Eu2+ ion-doped zeolite was formed, and the temperature measurement was performed in combination with a laser, a spectrometer and a filter.
It improves the sensitivity of fiber optic temperature sensors, can work stably in complex electromagnetic environments, expands the scope of application, and enhances safety in flammable and explosive environments.
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Figure CN120489370A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the field of optical fiber sensors, and in particular relates to a Eu 2+ Fiber optic temperature sensor prepared by ion-doped zeolite. Background Art
[0002] Temperature, as a key physical parameter, plays a vital role in numerous fields, including industrial production, scientific research, and healthcare. Accurate temperature measurement is crucial for these applications. While traditional temperature sensors, such as thermocouples and thermistors, meet common temperature measurement needs to a certain extent, they suffer from several significant drawbacks. Thermocouples are susceptible to electromagnetic interference, significantly reducing measurement accuracy in strong electromagnetic environments. Thermistors have a relatively narrow measurement range, and their stability and reliability require further improvement. These traditional sensors exhibit significant limitations in specific application scenarios. In high-voltage power equipment, due to strong electric and magnetic fields, thermocouples and thermistors cannot accurately measure temperature and can be damaged by electromagnetic interference. Furthermore, in flammable and explosive environments, the electrical characteristics of traditional sensors can pose safety risks.
[0003] Combining optical fibers with fluorescent materials to design fluorescent fiber temperature sensors is a key research area. The luminescence properties of fluorescent materials vary with temperature, and these changes are coupled into the optical fiber transmission. By analyzing the fluorescent signal emitted by the optical fiber, temperature information can be obtained. This design allows the sensor to remain stable in complex electromagnetic environments, expanding its application range.
[0004] At present, many rare earth ions have been used as fluorescent fiber temperature sensors, such as Yb 3+ 、Er 3+ 、Ce 3+ 、Eu 3+ Plasma-doped crystals exhibit photoluminescence properties. Temperature changes can influence the intensity of their luminescence, thereby obtaining temperature parameters. This, to a certain extent, meets the detection needs of various scenarios. However, compared to +3-valent rare earth ions, the outer electron structure of +2-valent rare earth ions makes them more susceptible to environmental influences. This high sensitivity to environmental changes translates into significant advantages at the sensor level. Therefore, the development of +2-valent rare earth ion fiber temperature sensors is of great significance. Summary of the Invention
[0005] Based on the above shortcomings of the prior art, the present invention provides a Eu 2+ Fiber optic temperature sensor prepared by ion-doped zeolite. Eu was obtained by high-temperature reduction method. 2+Ion-doped zeolite material is compounded with resin and then coated on the end of the optical fiber to obtain an optical fiber temperature sensor. 3+ The optical fiber temperature sensor is made of ion-doped zeolite material and has higher sensitivity.
[0006] To achieve the above object, the present invention provides the following technical solutions: A kind of Eu 2+ An optical fiber temperature sensor made of ion-doped zeolite, comprising an optical fiber sensor probe, a laser, a spectrometer, an optical filter, and a computer; The optical fiber sensor probe is composed of an optical fiber and a fluorescent material, and the fluorescent material is coated on the end of the optical fiber; The laser can emit 365nm laser light; The filter can block light with a wavelength less than 450nm from passing through.
[0007] As a Eu 2+ Further preference is given to optical fiber temperature sensors prepared from ion-doped zeolite.
[0008] Preferably, the method for preparing the fluorescent material coated on the end of the optical fiber comprises the following steps: S1. Grind 3A zeolite and europium oxide in a mortar for 40-60 minutes to obtain a mixed powder; S2. Place the mixed powder in step S1 in a tube furnace, introduce a mixture of H2 / N2 (volume ratio 1:10), and heat for 3 hours; S3, grinding the mixed powder heated in step S2 in a vacuum oven for 40-60 minutes; S4, adding the powder ground in step S3 to a mixed solution of glycerol, isopropyl alcohol, pentaerythritol triacrylate and hydroxycyclohexyl phenyl ketone, and stirring for 5-10 minutes to obtain a coating solution; S5, the coating solution obtained in step S4 is applied to the front end of the optical fiber by the dip-coating method, and finally 400mJ / cm 2 UV curing.
[0009] Preferably, the added amounts of 3A zeolite and europium oxide in step S1 are 0.5-1 g and 0.01-0.03 g, respectively.
[0010] Preferably, the heating temperature in step S2 is 300-400°C.
[0011] Preferably, the stirring speed in step S4 is 3000-4000 r / min.
[0012] Preferably, the amounts of glycerol, ethanol, pentaerythritol triacrylate and hydroxycyclohexyl phenyl ketone added in step S4 are 3-6 mL, 50-100 mL, 0.2-1 mL and 0.05-0.25 mL, respectively.
[0013] The beneficial effects of the present invention compared to the prior art are: (1) Compared with +3 valence Eu 3+ Fiber optic temperature sensor prepared by ion-doped zeolite, +2-valent Eu 2+ The optical fiber temperature sensor made of ion-doped zeolite has higher sensitivity.
[0014] (2) In the preferred embodiment, a stirring speed of 3000-4000 r / min can form a coating solution, while a speed that is too low will cause the mixed powder to settle at the bottom of the sol.
[0015] (3) In the preferred embodiment, a heating temperature of 300~400℃ can obtain better luminous intensity. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 It is a structural diagram of the optical fiber temperature sensor; Figure 2 Eu prepared in Example 1 2+ EDS spectrum of ion-doped zeolite; Figure 3 is the fluorescence emission spectrum of the fluorescent materials prepared in Example 1 and Comparative Example 1; Figure 4 is the fluorescence emission spectra of the fluorescent materials prepared in Examples 1-3 and Comparative Examples 3-4; Figure 5 are photographs of the coating dispersions prepared in Example 1 and Comparative Example 5; Figure 6 is the fluorescence signal of the optical fiber temperature sensor in Example 1 tested at different temperatures; Figure 7 is the fluorescence signal of the optical fiber temperature sensor in Comparative Example 1 tested at different temperatures; Figure 8 The figure shows a comparison of the sensitivity of the optical fiber temperature sensors in Example 1 and Comparative Example 1. DETAILED DESCRIPTION
[0017] In order to make the objectives, technical solutions and advantages of the present invention more clear, the present invention is further described in detail below in conjunction with the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
[0018] The present invention is described below by means of specific examples and comparative examples. Example
[0019] This embodiment provides a Eu 2+ Fiber optic temperature sensor prepared by ion-doped zeolite.
[0020] The sensor includes a fiber optic sensor probe, a laser, a spectrometer, a filter and a computer; The optical fiber sensor probe is composed of an optical fiber and a fluorescent material, and the fluorescent material is coated on the end of the optical fiber; The laser can emit 365nm laser light; The filter can block light with a wavelength less than 450nm from passing through.
[0021] The method for preparing the fluorescent material coated on the end of the optical fiber comprises the following steps: S1. Grind 0.5 g of 3A zeolite and 0.01 g of europium oxide in a mortar for 40 min to obtain a mixed powder; S2. Place the mixed powder in step S1 in a tube furnace, introduce a mixture of H2 / N2 (volume ratio 1:10), and then heat at 400°C for 3h; S3, grinding the mixed powder heated in step S2 in a vacuum oven for 40 minutes; S4, adding the powder ground in step S3 to a mixed solution of 3 mL of glycerol, 50 mL of isopropyl alcohol, 0.2 mL of pentaerythritol triacrylate, and 0.05 mL of hydroxycyclohexyl phenyl ketone, while stirring at a speed of 3000 r / min for 5 min to obtain a coating solution; S5, the coating solution obtained in step S4 is applied to the front end of the optical fiber by the dip-coating method, and finally 400mJ / cm 2 UV curing. Example
[0022] This embodiment provides a Eu 2+ Fiber optic temperature sensor prepared by ion-doped zeolite.
[0023] The sensor includes a fiber optic sensor probe, a laser, a spectrometer, a filter and a computer; The optical fiber sensor probe is composed of an optical fiber and a fluorescent material, and the fluorescent material is coated on the end of the optical fiber; The laser can emit 365nm laser light; The filter can block light with a wavelength less than 450nm from passing through.
[0024] The method for preparing the fluorescent material coated on the end of the optical fiber comprises the following steps: S1. Grind 0.7 g of 3A zeolite and 0.02 g of europium oxide in a mortar for 50 min to obtain a mixed powder; S2. Place the mixed powder in step S1 in a tube furnace, introduce a mixture of H2 / N2 (volume ratio 1:10), and then heat at 350°C for 3h; S3, grinding the mixed powder heated in step S2 in a vacuum oven for 50 minutes; S4, adding the powder ground in step S3 to a mixed solution of 5 mL of glycerol, 70 mL of isopropyl alcohol, 0.5 mL of pentaerythritol triacrylate, and 0.1 mL of hydroxycyclohexyl phenyl ketone, while stirring at a speed of 3500 r / min for 7 minutes to obtain a coating solution; S5, the coating solution obtained in step S4 is applied to the front end of the optical fiber by the dip-coating method, and finally 400mJ / cm 2 UV curing. Example
[0025] This embodiment provides a Eu 2+ Fiber optic temperature sensor prepared by ion-doped zeolite.
[0026] The sensor includes a fiber optic sensor probe, a laser, a spectrometer, a filter, and a computer; The optical fiber sensor probe is composed of an optical fiber and a fluorescent material, and the fluorescent material is coated on the end of the optical fiber; The laser can emit 365nm laser light; The filter can block light with a wavelength less than 450nm from passing through.
[0027] The method for preparing the fluorescent material coated on the end of the optical fiber comprises the following steps: S1. Grind 1 g of 3A zeolite and 0.03 g of europium oxide in a mortar for 60 min to obtain a mixed powder; S2. Place the mixed powder in step S1 in a tube furnace, introduce a mixture of H2 / N2 (volume ratio 1:10), and then heat at 300°C for 3h; S3, grinding the mixed powder heated in step S2 in a vacuum oven for 60 minutes; S4, adding the powder ground in step S3 to a mixed solution of 6 mL of glycerol, 100 mL of isopropyl alcohol, 1 mL of pentaerythritol triacrylate, and 0.25 mL of hydroxycyclohexyl phenyl ketone, while stirring at a speed of 4000 r / min for 10 min to obtain a coating solution; S5, the coating solution obtained in step S4 is applied to the front end of the optical fiber by the dip-coating method, and finally 400mJ / cm 2 UV curing.
[0028] This comparative example provides a Eu 3+ Fiber optic temperature sensor prepared by ion-doped zeolite.
[0029] The difference between this comparative example and Example 1 is that no H2 / N2 (volume ratio 1:10) mixed gas is introduced during the heating process described in step S2.
[0030] This comparative example provides a Eu 3+ Fiber optic temperature sensor prepared by ion-doped zeolite.
[0031] The difference between this comparative example and Example 1 is that the filter can block light with a wavelength less than 400 nm from passing through.
[0032] This embodiment provides a Eu 2+ Fiber optic temperature sensor prepared by ion-doped zeolite.
[0033] The difference between this comparative example and Example 1 is that the heating temperature in step S2 is 100°C.
[0034] This embodiment provides a Eu 2+ Fiber optic temperature sensor prepared by ion-doped zeolite.
[0035] The difference between this comparative example and Example 1 is that the heating temperature in step S2 is 200°C.
[0036] This embodiment provides a Eu 2+ Fiber optic temperature sensor prepared by ion-doped zeolite.
[0037] The difference between this comparative example and Example 1 is that the stirring speed in step S4 is 1000 r / min.
[0038] The innovation of the present invention is demonstrated in detail below with reference to the accompanying drawings. Figure 1 This is a structural diagram of the fiber optic temperature sensor. It can be seen that the sensor includes a fiber optic sensor probe, a laser, a spectrometer, a filter and a computer.
[0039] Figure 2 Eu prepared in Example 1 2+ EDS spectrum of ion-doped zeolite, which shows that the prepared fluorescent material contains rare earth element Eu.
[0040] Figure 3 The fluorescence emission spectra of the fluorescent materials prepared in Example 1 and Comparative Example 1 are shown. It can be seen that in the comparative example, no reducing gas H2 was introduced, and the emission peak was at around 610 nm, which is Eu 3+ions, and after reduction, the position of the emission peak of Example 1 changed, which indicates that Eu 3+ ions have been reduced to Eu 2+ ion.
[0041] Figure 4 The fluorescence emission spectra of the fluorescent materials prepared in Examples 1-3 and Comparative Examples 3-4 are shown. From the test results of the Examples and Comparative Examples, the intensity of the emitted light at a temperature of 300-400°C is significantly stronger than that at a temperature of 100-200°C.
[0042] Figure 5 The following are photos of the coating dispersions prepared in Example 1 and Comparative Example 5. The comparison shows that when the stirring speed is too slow, the fluorescent material is difficult to fully disperse in the resin, resulting in difficulty in obtaining a uniform coating. However, a rotation speed of 3000 r / min, as in the example, allows the fluorescent material to be dispersed in the solution.
[0043] Figure 6 and Figure 7 The following are the fluorescence signals of the optical fiber temperature sensors in Example 1 and Comparative Example 1 tested at different temperatures. By testing the signal strength of the optical fiber temperature sensors at 50°C, 100°C, 150°C, and 200°C, it can be seen that temperature can change the intensity of the output signal, indicating that temperature changes can be inferred from the output signal intensity. Furthermore, the peak value in Example 1 changes more significantly with temperature, indicating its better sensitivity.
[0044] Figure 8 The sensitivity of the optical fiber temperature sensor in Example 1 and Comparative Example 1 is compared. To further determine its sensitivity, a function curve is plotted using the peak values of Example 1 and Comparative Example 1. It can be seen more intuitively from the slope that the optical fiber temperature sensor in Example 1 has better sensitivity.
[0045] Those skilled in the art will appreciate that the foregoing descriptions are merely specific embodiments of the present invention, and not exhaustive. It should be noted that numerous variations and modifications are possible for those skilled in the art, and all such variations and modifications that do not exceed the scope of the claims should be considered within the scope of protection of the present invention.
Claims
1. A kind of Eu 2+ The optical fiber temperature sensor prepared by ion-doped zeolite is characterized in that: The optical fiber temperature sensor includes an optical fiber sensor probe, a laser, a spectrometer, an optical filter and a computer; The optical fiber sensor probe is composed of an optical fiber and a fluorescent material, and the fluorescent material is coated on the end of the optical fiber; The laser can emit 365nm laser light; The filter can block light with a wavelength less than 450nm from passing through.
2. The method for preparing the fluorescent material coated on the end of an optical fiber according to claim 1, comprising the following steps: S1. Grind 3A zeolite and europium oxide in a mortar for 40-60 minutes to obtain a mixed powder; S2. Place the mixed powder in step S1 in a tube furnace, introduce a mixture of H2 / N2 (volume ratio 1:10), and heat for 3 hours; S3, grinding the mixed powder heated in step S2 in a vacuum oven for 40-60 minutes; S4, adding the powder ground in step S3 to a mixed solution of glycerol, isopropyl alcohol, pentaerythritol triacrylate and hydroxycyclohexyl phenyl ketone, and stirring for 5-10 minutes to obtain a coating solution; S5, the coating solution obtained in step S4 is applied to the front end of the optical fiber by the dip-coating method, and finally 400 mJ / cm 2 UV curing.
3. The method for preparing the fluorescent material coated on the end of the optical fiber according to claim 2, characterized in that The added amounts of 3A zeolite and europium oxide in step S1 are 0.5-1 g and 0.01-0.03 g, respectively.
4. The method for preparing the fluorescent material coated on the end of the optical fiber according to claim 2, characterized in that The heating temperature in step S2 is 300-400°C.
5. The method for preparing the fluorescent material coated on the end of the optical fiber according to claim 2, characterized in that The stirring speed described in step S4 is 3000~4000r / min.
6. The method for preparing the fluorescent material coated on the end of an optical fiber according to claim 2, characterized in that The amounts of glycerol, ethanol, pentaerythritol triacrylate, and hydroxycyclohexyl phenyl ketone added in step S4 are 3-6 mL, 50-100 mL, 0.2-1 mL, and 0.05-0.25 mL, respectively.