Photochromic ceramic material and its use in laser power monitoring

Abstract

The application discloses a photochromic ceramic material and application thereof in laser power monitoring. 2.9‑x Na x Nb5O 15 :0.05Yb,0.05Er, wherein x=0.25-1.5. The material has a fast photochromic performance under 365nm irradiation, and different color change phenomena can be generated by irradiation of 980nm laser with different powers. By comparing the photochromic contrast with a pre-stored standard reference value (i.e. a predetermined relationship between laser power and photochromic contrast), real-time monitoring and display of laser power output can be realized.

Description

Technical Field

[0001] This invention belongs to the field of solid-state luminescent materials, specifically relating to a photochromic ceramic material and its application in laser power monitoring. Background Technology

[0002] Laser power monitoring is a crucial technology in laser applications, widely used in laser processing, laser medicine, optical communication, and scientific research. Accurate laser power monitoring not only ensures the stable operation of laser equipment but also guarantees processing precision, treatment effectiveness, and the reliability of experimental data. Currently, mainstream laser power monitoring technologies include pyroelectric detection, photodiode detection, and calorimetric detection. These traditional technologies generally suffer from problems such as difficulty in balancing response speed and monitoring accuracy, limited applicable wavelength range, poor tolerance to strong light, and insufficient long-term stability, failing to fully meet the high power monitoring requirements of modern laser technology. Furthermore, existing technologies also have shortcomings such as insufficient response speed and real-time performance, and a lack of integrated adjustment capabilities. Therefore, it is necessary to explore a new laser monitoring technology, providing a novel technical approach for laser power monitoring. Summary of the Invention

[0003] The purpose of this invention is to provide a photochromic ceramic material and its application in laser power monitoring. This ceramic material has a reverse reaction of photochromic effect based on the principle of thermosensitivity, that is, the "fading / recovery" process of photochromism can be driven by temperature to realize the monitoring of laser power. Therefore, it is expected to become a new material that can be applied to high-sensitivity laser power monitoring.

[0004] To achieve the above objectives, the present invention adopts the following technical solution: A photochromic ceramic material with the general chemical formula Sr 2.9-x Na x Nb5O 15 :0.05Yb,0.05Er, where x=0.25~1.5.

[0005] Specifically, the chemical formula of the ceramic material is: Sr 2.65 Na 0.25 Nb5O 15 0.05Yb, 0.05Er, Sr 2.4 Na 0.5 Nb5O 15 0.05Yb, 0.05Er, Sr 2.15 Na 0.75 Nb5O 15 0.05Yb, 0.05Er, Sr 1.9 NaNb5O 150.05Yb, 0.05Er, Sr 1.65 Na 1.25 Nb5O 15 0.05Yb, 0.05Er, Sr 1.4 Na 1.5 Nb5O 15 0.05Yb, 0.05Er. Sr is preferred. 1.9 NaNb5O 15 :0.05Yb,0.05Er.

[0006] Furthermore, the photochromic ceramic material is prepared by mixing raw materials containing SrCO3, Na2CO3, Nb2O5, Yb2O3 and Er2O3 according to the elemental stoichiometric ratio, and then pre-sintering and sintering.

[0007] Furthermore, the pre-sintering temperature is 960~1060℃, and the time is 3~7h.

[0008] Furthermore, the sintering temperature is 1280~1370℃, and the time is 2~6h.

[0009] The photochromic ceramic material can be used for laser power monitoring.

[0010] Under 365nm ultraviolet irradiation, the prepared photochromic ceramic material can achieve a rapid and high-performance photochromic effect. Subsequent irradiation with 980nm infrared light causes heat accumulation, leading to a localized temperature increase in the ceramic material and triggering a thermal bleaching effect in the phase change ceramic—specifically manifested as a characteristic recovery of its diffuse reflectance spectrum. Therefore, the testing system can use a signal detector to acquire spectral signals in real time, process and analyze the acquired signals, and calculate the photochromic contrast (the degree of photochromic change in the ceramic before and after irradiation). The obtained photochromic contrast is then compared with a pre-stored standard reference value (i.e., the established relationship between laser power and photochromic contrast), thereby achieving real-time monitoring and display of laser power output.

[0011] Furthermore, the monitored laser power ranged from 0 to 2.4 W.

[0012] The beneficial effects of this invention are as follows: This invention provides a sodium strontium niobate ceramic material that can achieve photochromic effects with 365nm irradiation and utilize the thermosensitive-mediated reverse photochromic reaction for laser power monitoring. This material exhibits excellent photochromic effects and rapid laser power monitoring characteristics, and its preparation process is simple and inexpensive, showing promising prospects for widespread application. Attached Figure Description

[0013] Figure 1 The X-ray diffraction pattern of the photochromic ceramic material prepared in Example 1 is shown.

[0014] Figure 2 This is a transmission electron microscope (TEM) image of the photochromic ceramic material prepared in Example 2.

[0015] Figure 3 The image shows the ultraviolet diffuse reflectance spectrum of the photochromic ceramic material prepared in Example 2 before and after 30 seconds of irradiation with a 365nm light source.

[0016] Figure 4 The graph shows the change in ultraviolet diffuse reflectance spectrum absorption intensity of the photochromic ceramic material prepared in Example 2 after irradiation with a 365nm light source for 30 seconds and heating at 300°C for 1 minute, repeated 10 times.

[0017] Figure 5 The color change of the photochromic ceramic material prepared in Example 2 after 30 seconds of irradiation with a 365nm light source and 3 minutes of irradiation with a 980nm light source of different powers is shown.

[0018] Figure 6 The photochromic ceramic material prepared in Example 2 undergoes a photochromic reaction under 365 nm irradiation, followed by ultraviolet diffuse reflectance spectra after being irradiated for 3 min by 980 nm light sources of different powers.

[0019] Figure 7 The graph (a) shows the curve relationship between different laser powers at 980nm and photochromic contrast through function fitting, and the bar graph (b) shows the calibrated standard values.

[0020] Figure 8 A schematic diagram illustrating the working principle of laser power measurement using the photochromic ceramic material of this invention. Detailed Implementation

[0021] To make the content of this invention easier to understand, the technical solution of this invention will be further described below with reference to specific embodiments, but this invention is not limited thereto.

[0022] Example 1. Preparation of photochromic ceramic materials Analytical-pure SrCO3, Nb2O5, Na2CO3, Yb2O3, and Er2O3 powders were precisely weighed according to the required elemental molar ratio. The weighed powders were then placed in an agate mortar, and anhydrous ethanol was added to grind them until uniformly mixed. The resulting refined particles were then placed in an alumina crucible and placed in a muffle furnace, heated to 1000℃, and held at that temperature for 4 hours for pre-sintering. The powders were then placed back in the agate mortar, ground with anhydrous ethanol to refine the powders, and finally sintered in a muffle furnace at 1360℃ for 2 hours to synthesize Sr.2.9-x Na x Nb5O 15 :0.05Yb,0.05Er (x=0.25, 0.5, 0.75, 1.0, 1.25, 1.5) ceramic materials, the sintered ceramic materials are further ground into powder.

[0023] Figure 1 The image shows the X-ray diffraction pattern of the prepared photochromic ceramic material. The data in the image indicate that the obtained photochromic ceramic material is similar to Sr₂NaNb₅O₂. 15 The PDF card is consistent with the original, proving that it is a pure phase and that no second phase was generated. Example 2

[0024] Accurately weigh 2.8049g SrCO3, 6.6453g Nb2O5, 0.5300g Na2CO3, 0.0985g Yb2O3, and 0.0956g Er2O3. Add anhydrous ethanol to an agate mortar and grind until uniformly mixed. Then, place the resulting refined particles in an alumina crucible and place it in a muffle furnace. Heat to 1000℃ and hold for 4 hours for pre-sintering. Next, place the powder in an agate mortar, add anhydrous ethanol, grind to refine the powder, and then sinter in a muffle furnace at 1360℃ for 2 hours to synthesize SrCO3. 1.9 NaNb5O 15 0.05Yb,0.05Er ceramic materials, the sintered ceramic materials are further ground into powder.

[0025] Figure 2 The image shows a scanning electron microscope (SEM) image of the prepared photochromic ceramic material. The image indicates that the sintered particles are uniform and exhibit good ceramic-like properties.

[0026] Figure 3 The image shows the ultraviolet diffuse reflectance spectrum of the prepared photochromic ceramic material before and after 30 seconds of irradiation with a 365nm light source. As can be seen from the image, the ceramic material exhibits strong absorption in the visible light region after 30 seconds of irradiation with a 365nm light source, and its photochromic efficiency can reach 47.67%.

[0027] Figure 4 The graph shows the change in ultraviolet diffuse reflectance absorption intensity of the prepared photochromic ceramic material after 10 cycles of irradiation with a 365nm light source for 30 seconds and heating at 300℃ for 1 minute. As shown in the figure, the change in ultraviolet diffuse reflectance absorption intensity of the ceramic material after irradiation with a 365nm light source for 30 seconds and heating at 300℃ for 1 minute is stable, proving that it has good cyclic stability.

[0028] Figure 5The image shows the color change of the prepared photochromic ceramic material after irradiation with a 365 nm light source for 30 seconds, followed by irradiation with 980 nm laser sources of different powers for 3 minutes (characterized under focused and diffused beam irradiation conditions, respectively). As can be seen from the figure, with the increase of 980 nm laser power (0→2.4W), the sample exhibits a gradual fading phenomenon, accompanied by a gradually clearer color transition from dark to light.

[0029] Figure 6 The image shows the ultraviolet diffuse reflectance spectra of the prepared photochromic ceramic material after photochromic reaction at 365 nm and subsequent irradiation for 3 minutes with 980 nm light sources of different powers. As can be seen from the figure, the intensity of the ultraviolet diffuse reflectance spectrum of the ceramic material significantly decreases after 365 nm irradiation. However, after 3 minutes of irradiation with 980 nm light sources of different powers, the intensity of the ultraviolet diffuse reflectance gradually increases with increasing 980 nm light source power. This demonstrates that irradiation with a 980 nm light source possesses a photothermal-driven bleaching effect, and the higher the light power, the better the bleaching effect.

[0030] Furthermore, a curve relationship was established between different laser powers at 980nm and photochromic efficiency through function fitting, resulting in a graph showing the relationship between photochromic contrast ratio ΔRt (i.e., the degree of photochromic change) and laser power. Figure 7 As shown, the trend of photochromic contrast with laser power can be well fitted by a function: The study confirmed that laser power has a significant regulatory effect on ΔRt: in the range of 0.4-2.4W, ΔRt decreased from 42.33% to 23.02%, and when it exceeded 2.4W, ΔRt reached saturation (23.02%), which is close to the upper limit of dose detection.

[0031] The above experiments show that the photochromic contrast ratio ΔRt is directly related to the degree of color change. Therefore, using ΔRt as a characteristic response parameter of 980 nm laser power can quantitatively characterize the relationship between laser power and the degree of color change. Based on this, this invention is the first to apply the photochromic effect to laser power monitoring. Figure 8 This demonstrates the working principle of photochromic ceramics using their thermosensitive properties to measure laser power: under laser irradiation, the pre-colored ceramic material (based on UV coloring) changes color due to Yb... 3+ Near-infrared absorption and ultraviolet radiation generate heat, leading to heat storage. This heat accumulation raises the local temperature, causing thermal bleaching of the ceramic material, which induces a characteristic recovery in its diffuse reflectance spectrum. The testing system can acquire spectral signals in real time through a signal detector, then process and analyze the acquired signals using built-in programs, and calculate the change in the degree of photochromism—the photochromic contrast ratio ΔRt. This ΔRt is then compared with a standard reference value (i.e.,...). Figure 7The fitting equation is compared to the actual equation to achieve real-time monitoring and display of laser power output.

[0032] The above description is only a preferred embodiment of the present invention. All equivalent changes and modifications made within the scope of the claims of the present invention should be included in the scope of the present invention.

Claims

1. A photochromic ceramic material, characterized in that, The general chemical formula of the ceramic material is Sr. 2.9- x Na x Nb5O 15 :0.05Yb,0.05Er, where x=0.25~1.

5.

2. The photochromic ceramic material according to claim 1, characterized in that, The specific chemical formula of the ceramic material is: Sr 2.65 Na 0.25 Nb5O 15 0.05Yb, 0.05Er, Sr 2.4 Na 0.5 Nb5O 15 0.05Yb, 0.05Er, Sr 2.15 Na 0.75 Nb5O 15 0.05Yb, 0.05Er, Sr 1.9 NaNb5O 15 0.05Yb, 0.05Er, Sr 1.65 Na 1.25 Nb5O 15 0.05Yb, 0.05Er, Sr 1.4 Na 1.5 Nb5O 15 :0.05Yb,0.05Er.

3. The photochromic ceramic material according to claim 1 or 2, characterized in that, Its preparation involves mixing raw materials SrCO3, Na2CO3, Nb2O5, Yb2O3 and Er2O3 according to the elemental stoichiometric ratio, and then obtaining the product through pre-sintering and sintering.

4. The photochromic ceramic material according to claim 3, characterized in that, The pre-sintering temperature is 960~1060℃, and the time is 3~7h.

5. The photochromic ceramic material according to claim 3, characterized in that, The sintering temperature is 1280~1370℃, and the time is 2~6h.

6. The application of a photochromic ceramic material as described in claim 1 or 2 in laser power monitoring, characterized in that, Under irradiation by a 365nm light source, the photochromic ceramic material can rapidly undergo a photochromic effect. Subsequently, irradiation with a 980nm light source will induce a thermal bleaching effect in the ceramic material. Therefore, by using a signal detector to collect spectral signals in real time and calculate the photochromic contrast, and then comparing the obtained photochromic contrast with a pre-stored standard reference value, real-time monitoring and display of laser power output can be achieved.

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