Phosphate laser neodymium glass and method of making same

CN122748918APending Publication Date: 2026-09-15LONGGUANGTIANXU SOLAR ENERGY ZHUCHENG
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Patent Information

Application Number
CN202611053161.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-07-15
Publication Date
2026-09-15

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Abstract

The application discloses a phosphate laser neodymium glass and a preparation method thereof, and belongs to the technical field of laser glasses. The phosphate laser neodymium glass is prepared from raw materials including P2O5 41-58 mol%, Al2O3 7-14 mol%, K2O 9-16 mol%, BaO 8-13 mol%, MgO 3-7 mol%, Nd2O3 0.6-3 mol%, Ga2O3 1-4 mol%, Nb2O5 0.8-3 mol%, ZnO 2-5 mol%, Sb2O3 0.1-1 mol%, KMg3(AlSi3O 10 )F 2 2.1-4.5 mol% in terms of mol percentage. The phosphate laser neodymium glass prepared by the method has high mechanical strength and high laser damage threshold.
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Description

Technical Field

[0001] This invention discloses a phosphate laser neodymium glass and its preparation method, belonging to the field of laser glass technology. Background Technology

[0002] Neodymium phosphate (Nd:P phosphate) laser glass, as a core gain medium in high-power laser systems, plays an irreplaceable role in fields such as inertial confinement fusion, laser ranging, medical lasers, and national defense. As laser technology advances towards higher power and higher energy, increasingly stringent requirements are being placed on the performance of Nd:P phosphate laser glass, primarily including high stimulated emission cross-section, low nonlinear refractive index, good thermal stability, high mechanical strength, and resistance to laser damage.

[0003] Currently, existing phosphate laser neodymium glass mainly consists of P2O5 as the network forging body, supplemented with Al2O3, alkali metal oxides, alkaline earth metal oxides, and Nd2O3. The Vickers hardness of traditional phosphate laser neodymium glass is generally below 500 HV, making it prone to cracking and wear during processing, transportation, and use, thus limiting its application in large-scale laser devices. Furthermore, the laser damage threshold of existing phosphate laser neodymium glass is typically below 10 J / cm². 2 Laser damage can easily occur under prolonged, repeated high-power laser pumping, affecting the lifespan and stability of the laser system. Current fabrication processes often employ high-temperature melting or annealing in a CCl4 atmosphere. During this process, chloride ions replace hydroxyl groups to generate HCl, which then volatilizes, but residual Cl remains. - The potential for damage to glass can affect its photoelectric properties. Although these existing technologies have achieved some success in practical applications, problems remain, such as insufficient mechanical strength, low laser damage threshold, and the need for optimization of the fabrication process. Summary of the Invention

[0004] To address the aforementioned problems in the prior art, this invention provides a phosphate laser neodymium glass and its preparation method, achieving the following objectives: This improves the thermal stability, mechanical strength, and photoelectric properties of glass, while shortening the production cycle and increasing production efficiency.

[0005] To achieve the above objectives, the following technical solution is adopted: A phosphate laser neodymium glass, comprising, by molar percentage: P₂O₅ 41~58 mol%, Al₂O₃ 7~14 mol%, K₂O 9~16 mol%, BaO 8~13 mol%, MgO 3~7 mol%, Nd₂O₃ 0.6~3 mol%, Ga₂O₃ 1~4 mol%, Nb₂O₅ 0.8~3 mol%, ZnO 2~5 mol%, Sb₂O₃ 0.1~1 mol%, and fluorocrystalline mica (KMg₃(AlSi₃O₄)₂).10 )F2)2.1~4.5mol%.

[0006] P2O5: As a network formant in glass, it provides the basic structural framework of glass. Too high a content will lead to a decrease in the chemical stability of glass, while too low a content will affect the glass forming ability.

[0007] Al2O3 can improve the network structure of glass, enhance its chemical stability and mechanical strength, and inhibit crystallization.

[0008] K2O: As a network modifier, it can lower the melting temperature of glass, improve the fluidity of glass, and adjust the refractive index of glass.

[0009] BaO: It can improve the chemical and thermal stability of glass, but excessive content will lead to an increase in the tendency of glass to crystallize.

[0010] MgO: can improve the mechanical strength and chemical stability of glass, while reducing the coefficient of thermal expansion of glass.

[0011] Nd₂O₃: As an activating ion, it is a key component for laser generation, and its content directly affects the laser performance of the glass. In this invention, the Nd₂O₃ content is 0.6~3 mol%, and within this range, high laser gain can be obtained without concentration quenching.

[0012] Ga2O3 can significantly improve the mechanical strength and chemical stability of glass, while also improving its optical uniformity. 3+ Ions can partially replace Al 3+ Ions enter the glass network, enhancing the stability of the network structure.

[0013] Nb₂O₅: Possesses a high refractive index and excellent optical properties, which can improve the laser damage threshold of glass and modulate its dispersion characteristics. The synergistic effect of Nb₂O₅ and Ga₂O₃ can significantly enhance the overall performance of glass.

[0014] ZnO: It can lower the melting temperature of glass, improve the forming properties of glass, and enhance the chemical stability of glass.

[0015] Sb2O3: It can effectively remove air bubbles in molten glass and is used as a clarifying agent to improve the transparency of glass.

[0016] Fluorocrystalline mica (KMg3(AlSi3O) 10 F2): It can significantly reduce the risk of thermal deformation of glass in high-temperature environments and suppress thermal damage caused by laser pumping.

[0017] A method for preparing phosphate laser neodymium glass includes the following steps: I. Grinding of Powder Weigh the raw materials of each component according to the above molar ratio, put the weighed raw materials into a planetary ball mill, grind for 30~45 minutes, and mix evenly to obtain a mixed powder.

[0018] II. Segmented Melting 1. Place the mixed powder into a crucible and put it into a heating furnace. First, continuously introduce nitrogen gas into the heating furnace at a flow rate of 2~5L / min, and keep it at the temperature for 1~2 hours. The temperature for keeping it at the temperature for 650~750℃. 2. The preheated mixture powder is heated to 1250~1350℃ to obtain molten glass. A mixture of nitrogen trifluoride and nitrogen is continuously introduced into the molten glass, and the molten glass is stirred at a stirring rate of 80 r / min for 2~3 h. The volume ratio of nitrogen trifluoride to nitrogen in the mixed gas is 1:(15~20), and the total flow rate is 4~6 L / min.

[0019] 3. Continuously introduce pure oxygen into the molten glass and raise the temperature to 1400~1500℃. The pure oxygen flow rate is 4~6L / min. After 1.5~2 hours, stop introducing pure oxygen and continue to maintain the temperature while subjecting the molten glass to ultrasonic treatment. The ultrasonic power is 500~800W, the frequency is 80~90kHz, and the ultrasonic treatment time is 20~40 minutes.

[0020] III. Molding Annealing The ultrasonically treated molten glass is poured into a mold preheated to 400-450℃ and allowed to stand for 20-30 minutes to solidify. The solidified glass, along with the mold, is then transferred to an annealing furnace. The temperature is first increased to 560-620℃ at a rate of 5-10℃ / min and held for 1-1.5 hours. Then, the temperature is decreased to 300-370℃ at a rate of 8-12℃ / min. The heat source is turned off, and the annealing furnace is kept sealed. After natural cooling to room temperature, the glass is demolded to obtain phosphate laser-treated neodymium glass.

[0021] The beneficial effects of this invention are as follows: The laser damage threshold of the phosphate-modified neodymium glass prepared by this invention is 13.5~15.8 J / cm. 2 Its glass transition temperature (Tg) is 672~706 ℃, and its Vickers hardness is 535HV~572 HV, indicating high mechanical strength and a high glass transition temperature, which can effectively resist thermal distortion and laser damage caused by repeated high-power laser pumping; the stimulated emission cross-section is 4.53~4.76×10 - 20 cm 2 This is beneficial for improving laser gain efficiency; the nonlinear refractive index is 0.48~1.11×10⁻⁶. -13ESU helps reduce the self-focusing effect of lasers at high power and improves the stability of the laser system. The fabrication process provided by this invention, through segmented atmosphere control, shortens the production cycle compared to traditional processes, while simultaneously improving the uniformity and photoelectric properties of the glass. The introduction of ultrasonic defoaming treatment during the fabrication process effectively eliminates bubbles in the molten glass, improving the uniformity and transparency of the glass. Detailed Implementation

[0022] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be described in further detail below. It should be understood that the specific embodiments described herein are for illustrative and explanatory purposes only and are not intended to limit the scope of the invention.

[0023] Example 1: A Phosphate Laser Neodymium Glass The molar percentage composition of a raw material for preparing phosphate laser neodymium glass includes: P2O551.9mol%, Al2O310mol%, K2O 12mol%, BaO 8mol%, MgO 6mol%, Nd2O31mol%, Ga2O33mol%, Nb2O51mol%, ZnO 4mol%, Sb2O30.1mol%, KMg3(AlSi3O 10 )F23mol%.

[0024] A method for preparing phosphate laser neodymium glass includes the following steps: I. Grinding of Powder Weigh the raw materials of each component according to the above molar ratio, put the weighed raw materials into a planetary ball mill, grind for 45 minutes, and mix evenly to obtain a mixed powder.

[0025] II. Segmented Melting 1. Place the mixed powder into a crucible and put it into a heating furnace. Preheat it for 1 hour at a temperature of 750℃. During the preheating process, nitrogen gas is continuously introduced into the mixed powder at a flow rate of 2L / min.

[0026] 2. The preheated mixed powder is heated to 1350℃ to obtain molten glass. A mixture of nitrogen trifluoride and nitrogen is continuously introduced into the molten glass, and the glass is stirred at a stirring rate of 80 r / min for 2 hours. The volume ratio of nitrogen trifluoride to nitrogen in the mixed gas is 1:15, and the total flow rate is 4 L / min.

[0027] 3. Continuously introduce pure oxygen into the molten glass and raise the temperature to 1400℃. After 1.5 hours, stop introducing pure oxygen and continue to hold the temperature while subjecting the molten glass to ultrasonic treatment. The pure oxygen flow rate is 4L / min, the ultrasonic power is 800W, the frequency is 90kHz, and the ultrasonic treatment time is 30 minutes.

[0028] III. Molding Annealing The ultrasonically treated molten glass was poured into a mold preheated to 450°C and allowed to stand for 30 minutes to solidify. The solidified glass, along with the mold, was then transferred to an annealing furnace. The furnace was first heated to 600°C at a rate of 5°C / min and held at that temperature for 1.5 hours. Then, the temperature was lowered to 350°C at a rate of 10°C / min. The heat source was turned off, and the annealing furnace was kept sealed. The glass was allowed to cool naturally to room temperature before demolding to obtain phosphate laser-treated neodymium glass.

[0029] Example 2: A Phosphate Laser Neodymium Glass The molar percentage composition of a raw material for preparing phosphate laser neodymium glass includes: P2O543.7mol%, Al2O311mol%, K2O 14mol%, BaO 12mol%, MgO 5mol%, Nd2O32mol%, Ga2O34mol%, Nb2O52mol%, ZnO 3mol%, Sb2O30.3mol%, KMg3(AlSi3O 10 )F23mol%.

[0030] A method for preparing phosphate laser neodymium glass includes the following steps: I. Grinding of Powder Weigh the raw materials of each component according to the above molar ratio, put the weighed raw materials into a planetary ball mill, grind for 30 minutes, and mix evenly to obtain a mixed powder.

[0031] II. Segmented Melting 1. Place the mixed powder into a crucible and put it into a heating furnace. Preheat it for 2 hours at a temperature of 650℃. During the preheating process, nitrogen gas is continuously introduced into the mixed powder at a flow rate of 5L / min.

[0032] 2. The preheated mixture powder is heated to 1300℃ to obtain molten glass. A mixture of nitrogen trifluoride and nitrogen is continuously introduced into the molten glass, and the glass is stirred at a stirring rate of 80 r / min for 2 hours. The volume ratio of nitrogen trifluoride to nitrogen in the mixture is 1:20, and the total flow rate is 4 L / min.

[0033] 3. Continuously introduce pure oxygen into the molten glass and raise the temperature to 1400℃. After 2 hours, stop introducing pure oxygen and continue to maintain the temperature while subjecting the molten glass to ultrasonic treatment. The pure oxygen flow rate is 5L / min, the ultrasonic power is 600W, the frequency is 90kHz, and the ultrasonic treatment time is 30min.

[0034] III. Molding Annealing The ultrasonically treated molten glass was poured into a mold preheated to 400°C and allowed to stand for 30 minutes to solidify. The solidified glass, along with the mold, was then transferred to an annealing furnace. The furnace was first heated to 560°C at a rate of 10°C / min and held for 1.5 hours. Then, the temperature was lowered to 350°C at a rate of 8°C / min. The heat source was turned off, and the annealing furnace was kept sealed. After natural cooling to room temperature, the glass was demolded to obtain phosphate laser-treated neodymium glass.

[0035] Example 3: A Phosphate Laser Neodymium Glass The molar percentage composition of a raw material for preparing phosphate laser neodymium glass includes: P2O554.3mol%, Al2O38mol%, K2O 9.5mol%, BaO 8mol%, MgO 7mol%, Nd2O30.8mol%, Ga2O32mol%, Nb2O51.2mol%, ZnO 5mol%, Sb2O30.7mol%, KMg3(AlSi3O 10 )F23.5mol%.

[0036] A method for preparing phosphate laser neodymium glass includes the following steps: I. Grinding of Powder Weigh the raw materials of each component according to the above molar ratio, put the weighed raw materials into a planetary ball mill, grind for 30 minutes, and mix evenly to obtain a mixed powder.

[0037] II. Segmented Melting 1. Place the mixed powder into a crucible and put it into a heating furnace. Preheat it for 1 hour at a temperature of 700℃. During the preheating process, nitrogen gas is continuously introduced into the mixed powder at a flow rate of 2L / min.

[0038] 2. The preheated mixed powder is heated to 1300℃ to obtain molten glass. A mixture of nitrogen trifluoride and nitrogen gas is continuously introduced into the molten glass, and the molten glass is stirred at a stirring rate of 80 r / min for 3 hours. The volume ratio of nitrogen trifluoride to nitrogen gas in the mixed gas is 1:20, and the total flow rate is 6 L / min.

[0039] 3. Continuously introduce pure oxygen into the molten glass and raise the temperature to 1400℃. After 1.5 hours, stop introducing pure oxygen and continue to hold the temperature while subjecting the molten glass to ultrasonic treatment. The pure oxygen flow rate is 4L / min, the ultrasonic power is 500W, the frequency is 90kHz, and the ultrasonic treatment time is 30 minutes.

[0040] III. Molding Annealing The ultrasonically treated molten glass was poured into a mold preheated to 450°C and allowed to stand for 20 minutes to solidify. The solidified glass, along with the mold, was then transferred to an annealing furnace. The furnace was first heated to 600°C at a rate of 5°C / min and held at that temperature for 1.5 hours. Then, the temperature was lowered to 300°C at a rate of 12°C / min. The heat source was turned off, and the annealing furnace was kept sealed. After natural cooling to room temperature, the glass was demolded to obtain phosphate laser-treated neodymium glass.

[0041] Example 4: A Phosphate Laser Neodymium Glass The molar percentage composition of a raw material for preparing phosphate laser neodymium glass includes: P2O551mol%, Al2O310mol%, K2O 13mol%, BaO 9mol%, MgO 4mol%, Nd2O31.5mol%, Ga2O33.5mol%, Nb2O51.4mol%, ZnO 4mol%, Sb2O30.5mol%, KMg3(AlSi3O 10 )F22.1mol%.

[0042] A method for preparing phosphate laser neodymium glass includes the following steps: I. Grinding of Powder Weigh the raw materials of each component according to the above molar ratio, put the weighed raw materials into a planetary ball mill, grind for 45 minutes, and mix evenly to obtain a mixed powder.

[0043] II. Segmented Melting 1. Place the mixed powder into a crucible and put it into a heating furnace. Keep it at a temperature of 750℃ for 2 hours. During the heat preservation process, nitrogen gas is continuously introduced into the mixed powder at a flow rate of 2L / min.

[0044] 2. The preheated mixture powder is heated to 1250℃ to obtain molten glass. A mixture of nitrogen trifluoride and nitrogen is continuously introduced into the molten glass, and the glass is stirred at a stirring rate of 80 r / min for 3 hours. The volume ratio of nitrogen trifluoride to nitrogen in the mixture is 1:15, and the total flow rate is 4 L / min.

[0045] 3. Continuously introduce pure oxygen into the molten glass and raise the temperature to 1500℃. After 1.5 hours, stop introducing pure oxygen and continue to hold the temperature while subjecting the molten glass to ultrasonic treatment. The pure oxygen flow rate is 6L / min, the ultrasonic power is 500W, the frequency is 80kHz, and the ultrasonic treatment time is 30 minutes.

[0046] III. Molding Annealing The ultrasonically treated molten glass is injected into a mold to form the glass. The mold is preheated to 450°C and coated with a release agent on its inner wall. The formed glass, along with the mold, is transferred into an annealing furnace. The temperature is first increased to 620°C at a rate of 10°C / min and held for 1 hour. Then, the temperature is decreased to 300°C at a rate of 8°C / min. The heat source is turned off, and the annealing furnace is kept sealed. After natural cooling to room temperature, the glass is demolded to obtain phosphate laser-treated neodymium glass.

[0047] Example 5: A Phosphate Laser Neodymium Glass A phosphate laser neodymium glass, the raw materials for which are prepared have a molar percentage composition comprising: P2O558mol%, Al2O37mol%, K2O 9mol%, BaO 9mol%, MgO 7mol%, Nd2O30.6mol%, Ga2O31.5mol%, Nb2O50.8mol%, ZnO 2.5mol%, Sb2O30.1mol%, KMg3(AlSi3O 10 )F24.5mol%.

[0048] A method for preparing phosphate laser neodymium glass includes the following steps: I. Grinding of Powder Weigh the raw materials of each component according to the above molar ratio, put the weighed raw materials into a planetary ball mill, grind for 30 minutes, and mix evenly to obtain a mixed powder.

[0049] II. Segmented Melting 1. Place the mixed powder into a crucible and put it into a heating furnace. Keep it at a temperature of 700℃ for 1 hour. During the heat preservation process, nitrogen gas is continuously introduced into the mixed powder at a flow rate of 5L / min.

[0050] 2. The preheated mixture powder is heated to 1350℃ to obtain molten glass. A mixture of nitrogen trifluoride and nitrogen is continuously introduced into the molten glass, and the glass is stirred at a stirring rate of 80 r / min for 3 hours. The volume ratio of nitrogen trifluoride to nitrogen in the mixture is 1:20, and the total flow rate is 6 L / min.

[0051] 3. Continuously introduce pure oxygen into the molten glass and raise the temperature to 1500℃. After 1.5 hours, stop introducing pure oxygen and continue to maintain the temperature while subjecting the molten glass to ultrasonic treatment. The pure oxygen flow rate is 4L / min, the ultrasonic power is 500W, the frequency is 80kHz, and the ultrasonic treatment time is 20min.

[0052] III. Molding Annealing The ultrasonically treated molten glass was poured into a mold preheated to 450°C and allowed to stand for 30 minutes to solidify. The solidified glass, along with the mold, was then transferred to an annealing furnace. The furnace was first heated to 600°C at a rate of 10°C / min and held for 1 hour. Then, the temperature was lowered to 370°C at a rate of 10°C / min. The heat source was turned off, and the annealing furnace was kept sealed. The glass was allowed to cool naturally to room temperature and then demolded to obtain phosphate laser-treated neodymium glass.

[0053] Example 6: A Phosphate Laser Neodymium Glass The molar percentage composition of a raw material for preparing phosphate laser neodymium glass includes: P2O541mol%, Al2O314mol%, K2O 16mol%, BaO 13mol%, MgO 3mol%, Nd2O33mol%, Ga2O31mol%, Nb2O53mol%, ZnO 2mol%, Sb2O31mol%, KMg3(AlSi3O 10 )F23mol%.

[0054] A method for preparing phosphate laser neodymium glass includes the following steps: I. Grinding of Powder Weigh the raw materials of each component according to the above molar ratio, put the weighed raw materials into a planetary ball mill, grind for 30 minutes, and mix evenly to obtain a mixed powder.

[0055] II. Segmented Melting 1. Place the mixed powder into a crucible and put it into a heating furnace. Preheat it for 2 hours at a temperature of 650℃. During the preheating process, nitrogen gas is continuously introduced into the mixed powder at a flow rate of 2L / min.

[0056] 2. The preheated mixture powder is heated to 1250℃ to obtain molten glass. A mixture of nitrogen trifluoride and nitrogen is continuously introduced into the molten glass, and the glass is stirred at a stirring rate of 80 r / min for 2 hours. The volume ratio of nitrogen trifluoride to nitrogen in the mixture is 1:15, and the total flow rate is 4 L / min.

[0057] 3. Continuously introduce pure oxygen into the molten glass and raise the temperature to 1500℃. After 1.5 hours, stop introducing pure oxygen and continue to hold the temperature while subjecting the molten glass to ultrasonic treatment. The pure oxygen flow rate is 4L / min, the ultrasonic power is 500W, the frequency is 90kHz, and the ultrasonic treatment time is 40min.

[0058] III. Molding Annealing The ultrasonically treated molten glass was poured into a mold preheated to 450°C and allowed to stand for 20 minutes to solidify. The solidified glass, along with the mold, was then transferred to an annealing furnace. The furnace was first heated to 560°C at a rate of 5°C / min and held for 1 hour. Then, the temperature was lowered to 350°C at a rate of 12°C / min. The heat source was turned off, and the annealing furnace was kept sealed. After natural cooling to room temperature, the glass was demolded to obtain phosphate laser-treated neodymium glass.

[0059] Comparative Example 1 The molar percentage composition of a raw material for preparing phosphate laser neodymium glass includes: P2O556.5mol%, Al2O310mol%, K2O 10mol%, BaO 9mol%, MgO 8mol%, Nd2O30.8mol%, ZnO 5mol%, Sb2O30.7mol%.

[0060] The laser-coated neodymium glass is prepared using the same method as the glass prepared in Example 1.

[0061] Comparative Example 2 The molar percentage composition of a raw material for preparing phosphate laser neodymium glass includes: P2O554.3mol%, Al2O38mol%, K2O 9.5mol%, BaO 8mol%, MgO 7mol%, Nd2O30.8mol%, Ga2O32mol%, Nb2O51.2mol%, ZnO 5mol%, Sb2O30.7mol%, KMg3(AlSi3O 10 )F23.5mol% A method for preparing phosphate laser neodymium glass includes the following steps: The mixed powder is placed in a crucible and then placed in a heating furnace. The temperature is controlled at 1250℃ to obtain molten glass. During the melting process, a mixture of O2 and CCl4 gas is introduced to bubble the molten glass for 3 hours. The volume ratio of O2 to CCl4 is 1:4.

[0062] After bubbling is completed, the glass melt is clarified and defoamed, with the temperature controlled at 1200℃ and kept at that temperature for 5 hours.

[0063] After the heat preservation is completed, the molten glass is stirred and poured into the mold for molding annealing to obtain neodymium glass. The molding annealing operation method is the same as the "molding annealing" step in Example 1.

[0064] Performance testing Glass performance tests were conducted on Examples 1-6 and Comparative Examples 1-2. The test methods are as follows, and the test results are shown in Table 1.

[0065] Nonlinear refractive index n2: The measurement was performed using Z-scan technology with a Ti:sapphire short-pulse laser, with the wavelength adjusted to 800 nm, pulse width to 100 fs, and repetition frequency to 1 kHz.

[0066] Stimulated emission cross section: Nd2 was measured using fluorescence spectroscopy with a fluorescence spectrophotometer. 3+ Ionic 4 F 3 / 2 → 4 I 11 / 2 The fluorescence spectrum of the transition was obtained, and the stimulated emission cross section was calculated according to the Fuchtbauer-Ladenburg equation.

[0067] Laser damage threshold: Referring to ISO 11254-1:2021, a 1064nm nanosecond laser pulse was used for testing, with a pulse width of 10ns, a repetition frequency of 10Hz, and an R-on-1 test mode. The test result is the damage threshold with a probability of 10%.

[0068] Vickers hardness: Refer to GB / T 4340.1-2009, use HV-1000 Vickers hardness tester, test load 500g, holding time 15s, test 5 points for each sample, and take the average value.

[0069] Glass transition temperature Tg: Tested by differential scanning calorimetry (DSC) according to ISO 11357-2:2020 standard; a differential scanning calorimeter was used, and the heating rate was controlled at 10℃ / min.

[0070] Table 1. Glass performance test results The data above show that the laser damage threshold of the phosphate laser-treated neodymium glass prepared in this invention is 13.5~15.8 J / cm. 2 Its glass transition temperature (Tg) is 672~706 ℃, and its Vickers hardness is 535HV~572 HV, indicating high mechanical strength and a high glass transition temperature, which can effectively resist thermal distortion and laser damage caused by repeated high-power laser pumping; the stimulated emission cross-section is 4.53~4.76×10⁻⁶. -20 cm 2 This is beneficial for improving laser gain efficiency; the nonlinear refractive index is 0.48~1.11×10⁻⁶. -13ESU helps reduce the self-focusing effect of lasers at high power and improves the stability of laser systems.

[0071] Obviously, there are many other possible implementation methods under the concept of this invention. It should be stated here that any changes made under the inventive concept of this invention will fall within the protection scope of this invention.

Claims

1. A phosphate laser neodymium glass, characterized in that: The raw material composition, by molar percentage, includes: P2O5 41~58 mol%, Al2O3 7~14 mol%, K2O 9~16 mol%, BaO 8~13 mol%, MgO 3~7 mol%, Nd2O3 0.6~3 mol%, Ga2O3 1~4 mol%, Nb2O5 0.8~3 mol%, ZnO 2~5 mol%, Sb2O3 0.1~1 mol%, and KMg3(AlSi3O) 10 F2 2.1~4.5mol%.

2. The method for preparing phosphate laser neodymium glass according to claim 1, characterized in that: The process includes powder grinding, segmented melting, and forming annealing steps; the powder grinding involves grinding P2O5, Al2O3, K2O, BaO, MgO, Nd2O3, Ga2O3, Nb2O5, ZnO, Sb2O3, and KMg3(AlSi3O) into powders. 10 Grind F2 for 30-45 minutes to obtain a mixed powder.

3. The method for preparing phosphate laser neodymium glass according to claim 2, characterized in that: The segmented melting process includes the following steps: S1. Place the mixed powder into a crucible and place it in a heating furnace for heat preservation and preheating, and continuously introduce nitrogen gas into the heating furnace at a flow rate of 2~5L / min; S2. The preheated mixed powder is heated to 1250~1350℃ to obtain molten glass. A mixture of nitrogen trifluoride and nitrogen is continuously introduced into the molten glass, and the molten glass is kept at the temperature and stirred for 2~3 hours. S3. Continuously introduce pure oxygen into the molten glass and raise the temperature to 1400~1500℃. After 1.5~2 hours, stop introducing pure oxygen and continue to keep the glass at the same temperature while performing ultrasonic treatment.

4. The method for preparing phosphate laser neodymium glass according to claim 3, characterized in that: The heat preservation and preheating process involves a heat preservation and preheating time of 1-2 hours and a heat preservation and preheating temperature of 650-750℃.

5. The method for preparing phosphate laser neodymium glass according to claim 3, characterized in that: In the mixed gas, the volume ratio of nitrogen trifluoride to nitrogen is 1:(15~20), and the total flow rate is 4~6L / min.

6. The method for preparing phosphate laser neodymium glass according to claim 3, characterized in that: The flow rate of the pure oxygen is 4~6 L / min.

7. The method for preparing phosphate laser neodymium glass according to claim 3, characterized in that: The ultrasonic treatment has an ultrasonic power of 500~800W, a frequency of 80~90kHz, and a processing time of 20~40min.

8. The method for preparing phosphate laser neodymium glass according to claim 2, characterized in that: The forming annealing process involves injecting ultrasonically treated molten glass into a preheated mold and allowing it to stand and form. The formed glass, along with the mold, is then transferred into an annealing furnace, heated to 560-620°C and held for 1-1.5 hours. The temperature is then lowered to 300-370°C, the heat source is turned off, and the glass is cooled and demolded to obtain phosphate laser neodymium glass.

9. The method for preparing phosphate laser neodymium glass according to claim 8, characterized in that: The heating rate is 5~10℃ / min; the cooling rate is 8~12℃ / min.

10. The method for preparing phosphate laser neodymium glass according to claim 8, characterized in that: Preheating: The mold is preheated to 400~450℃.