Magneto-optical glass with high transmittance and preparation method thereof

Abstract

The invention belongs to the field of glass manufacturing, and specifically relates to a high-transmittance magneto-optical glass and a preparation method thereof. The glass composition is: 10-30 parts of Tb4O7, 2-8 parts of Dy2O3, 5-15 parts of Ga2O3, 20-40 parts of B2O3, 5-20 parts of SiO2, 5-10 parts of Na2O, and 2-5 parts of K2O; 0.05%-0.25% of Sb2O3 is added to the above components, and then the magneto-optical glass with a transmittance of more than 70% in the visible light and near-infrared wavelength bands is prepared through the steps of batching, melting, bubbling, clarifying, stirring and homogenizing, molding, annealing, etc.

Description

Technical Field

[0001] The invention relates to the field of glass manufacturing, and in particular to a high-transmittance magneto-optical glass and a preparation method thereof. Background Art

[0002] Magneto-optical glass is widely used in optics, magnetism, communications and other technical fields. Magneto-optical isolators, magneto-optical switches, and other devices for controlling laser parameters have been developed. Therefore, the development of high-transmittance magneto-optical glass can effectively reduce the loss of laser in magneto-optical materials, improve the transmission efficiency of lasers, and increase the sensitivity of device use.

[0003] During the production process, Tb4O7 has a high melting point and is difficult to melt. Using a higher melting temperature will cause the electrons of certain impurity ions in the glass to transition, causing the glass to color and reduce the transmittance of the glass.

[0004] In the preparation process of conventional magneto-optical glass, the raw materials are generally made into a blank, which is then sintered and melted to make magneto-optical glass; or it is melted in a crucible and directly cast into shape; both methods do not involve stirring to eliminate unevenness in the glass, resulting in a large number of stripes in the glass, which affects the transmittance of the glass. Summary of the invention

[0005] The invention provides a magneto-optical glass with high transmittance and a preparation method thereof, and the magneto-optical glass with a transmittance of more than 70% in visible light and near infrared wavelength bands is prepared.

[0006] The present invention provides a magneto-optical glass with high transmittance, the glass composition of which is: 10-30 parts of Tb4O7, 2-8 parts of Dy2O3, 5-15 parts of Ga2O3, 20-40 parts of B2O3, 5-20 parts of SiO2, 5-10 parts of Na2O, 2-5 parts of K2O; 0.05wt.%-0.25wt.% of Sb2O3 is added to the above components.

[0007] The purity of the selected raw materials is above 99.99%, and the iron content of the raw materials is less than 5ppm.

[0008] The present application also provides a method for preparing the magneto-optical glass having high transmittance, comprising the following steps:

[0009] a) Ingredients: Calculate the raw materials required for the glass according to the glass composition, then weigh the raw materials and mix them evenly.

[0010] b) Melting: Place the mixture into a platinum crucible and place it into a silicon carbon rod electric furnace at 1200℃-1300℃ for 30-50min.

[0011] c) Bubbling: After the glass is melted, high-purity dry oxygen is introduced into the glass for 20-30 minutes to fully melt the raw materials.

[0012] d) Clarification: Stop the oxygen supply, raise the temperature of the electric furnace to 1400-1450°C, and carry out clarification to eliminate bubbles for 60-90 minutes.

[0013] e) Stirring and homogenizing: After clarification, cool the electric furnace to 1200-1250°C, place a platinum stirrer into the glass liquid for stirring, the stirring speed is 25-30r / min, the stirring time is 20-30min, and after stirring, let it stand for 10-20min.

[0014] f) Molding: Pour the glass liquid into the preheated mold quickly, and quickly put the glass into the muffle furnace. Set the temperature of the muffle furnace to 650-700℃ and keep it warm for 10 minutes.

[0015] g) Annealing: anneal at a rate of 15°C / hour to 300°C, then cool to 80°C at 30°C / hour, close the muffle furnace, and cool to room temperature.

[0016] The present invention has the following advantages:

[0017] 1. Through the glass composition and preparation method of the present invention, the transmittance of magneto-optical glass in visible light and near infrared can reach more than 70%, and the highest transmittance can reach 85%.

[0018] 2. By introducing Na2O and K2O, the melting temperature of glass is lowered, the difficulty of glass manufacturing is reduced, and the transmittance of magneto-optical glass is improved.

[0019] 3. Select high-purity raw materials to reduce the impact of impurities on the transmittance of magneto-optical glass.

[0020] 4. Use a platinum pot as a container to reduce the introduction of impurities during the smelting process and improve the glass transmittance.

[0021] 5. The present invention eliminates the stripes in the glass through the stirring process, reducing the influence of the stripes on the transmittance of the magneto-optical glass.

[0022] 6. The preparation process of the present invention is simple, the preparation efficiency is high, and batch production is possible. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 The transmittance curve of Example 1 is DETAILED DESCRIPTION

[0024] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0025] Example 1

[0026] A high-transmittance magneto-optical glass comprises: 15 parts of Tb4O7, 5 parts of Dy2O3, 10 parts of Ga2O3, 45 parts of B2O3, 15 parts of SiO2, 6 parts of Na2O, and 4 parts of K2O; 0.15% of Sb2O3 is added to the above components.

[0027] The purity of the raw materials used is above 99.99%, and the iron content of the raw materials is less than 5ppm.

[0028] The specific method for preparing glass includes the following steps:

[0029] Batching: Calculate the raw materials needed for the glass according to the glass composition, then weigh the raw materials and mix them evenly.

[0030] Melting: Place the mixture into a platinum crucible and place it into a silicon carbon rod electric furnace at 1280°C for 40 minutes.

[0031] Bubbling: After the glass is melted, high-purity dry oxygen is introduced into the glass for 30 minutes to fully melt the raw materials.

[0032] Clarification: Stop the oxygen supply, raise the temperature of the electric furnace to 1400℃, and carry out clarification to eliminate bubbles for 60 minutes.

[0033] Stirring and homogenizing: After clarification, the electric furnace is cooled to 1200°C, and a platinum stirrer is placed in the glass liquid for stirring. The stirring speed is 30r / min, and the stirring time is 30min. After stirring, let it stand for 15min.

[0034] Molding: Pour the glass liquid into the preheated mold quickly, and then quickly put the glass into the muffle furnace. Set the temperature of the muffle furnace to 650℃ and keep it warm for 10 minutes.

[0035] Annealing: anneal at a rate of 15°C / hour to 300°C, then cool to 80°C at 30°C / hour, close the muffle furnace and cool to room temperature.

[0036] The refractive index of the produced magneto-optical glass was tested, and the transmittance was higher than 70% in the wavelength range of 456nm-1594nm; the transmittance was the highest at a wavelength of 853nm, which was 86.1%.

[0037] Example 2

[0038] A high-transmittance magneto-optical glass comprises: 21 parts of Tb4O7, 4 parts of Dy2O3, 10 parts of Ga2O3, 42 parts of B2O3, 14 parts of SiO2, 6 parts of Na2O, and 3 parts of K2O; 0.15% of Sb2O3 is added to the above components.

[0039] The purity of the selected raw materials is above 99.99%, and the iron content of the raw materials is less than 5ppm.

[0040] The specific method for preparing glass includes the following steps:

[0041] Batching: Calculate the raw materials needed for the glass according to the glass composition, then weigh the raw materials and mix them evenly.

[0042] Melting: Place the mixture into a platinum crucible and place it into a silicon carbon rod electric furnace at 1280°C for 40 minutes.

[0043] Bubbling: After the glass is melted, high-purity dry oxygen is introduced into the glass for 30 minutes to fully melt the raw materials.

[0044] Clarification: Stop the oxygen supply, raise the temperature of the electric furnace to 1400℃, and carry out clarification to eliminate bubbles for 60 minutes.

[0045] Stirring and homogenizing: After clarification, the electric furnace is cooled to 1200°C, and a platinum stirrer is placed in the glass liquid for stirring. The stirring speed is 30r / min, and the stirring time is 30min. After stirring, let it stand for 15min.

[0046] Molding: Pour the glass liquid into the preheated mold quickly, and then quickly put the glass into the muffle furnace. Set the temperature of the muffle furnace to 650℃ and keep it warm for 10 minutes.

[0047] Annealing: anneal at a rate of 15°C / hour to 300°C, then cool to 80°C at 30°C / hour, close the muffle furnace and cool to room temperature.

[0048] The refractive index of the produced magneto-optical glass was tested, and the transmittance was higher than 70% in the wavelength range of 468nm-1585nm; the transmittance was the highest at a wavelength of 843nm, which was 84.9%.

[0049] Comparative Example 1

[0050] A high-transmittance magneto-optical glass comprises: 15 parts of Tb4O7, 5 parts of Dy2O3, 10 parts of Ga2O3, 45 parts of B2O3, 15 parts of SiO2, 4 parts of Na2O, and 4 parts of K2O; 0.15% of Sb2O3 is added to the above components.

[0051] The purity of the raw materials used is above 99.99%, and the iron content of the raw materials is less than 5ppm.

[0052] The specific method for preparing glass includes the following steps:

[0053] Batching: Calculate the raw materials needed for the glass according to the glass composition, then weigh the raw materials and mix them evenly.

[0054] Melting: Place the mixture into a platinum crucible and place it into a silicon carbon rod electric furnace at 1350°C for 60 minutes.

[0055] Bubbling: After the glass is melted, high-purity dry oxygen is introduced into the glass for 30 minutes to fully melt the raw materials.

[0056] Clarification: Stop the oxygen supply, raise the temperature of the electric furnace to 1400℃, and carry out clarification to eliminate bubbles for 60 minutes.

[0057] Stirring and homogenizing: After clarification, the electric furnace is cooled to 1200°C, and a platinum stirrer is placed in the glass liquid for stirring. The stirring speed is 30r / min, and the stirring time is 30min. After stirring, let it stand for 15min.

[0058] Molding: Pour the glass liquid into the preheated mold quickly, and then quickly put the glass into the muffle furnace. Set the temperature of the muffle furnace to 650℃ and keep it warm for 10 minutes.

[0059] Annealing: anneal at a rate of 15°C / hour to 300°C, then cool to 80°C at 30°C / hour, close the muffle furnace and cool to room temperature.

[0060] The refractive index of the produced magneto-optical glass was tested, and the transmittance was higher than 70% within the wavelength range of 653nm-1096nm; the transmittance was the highest at a wavelength of 843nm, reaching 76.3%.

[0061] By reducing the addition of Na2O in Example 1 and Comparative Example 1, the glass production temperature is significantly affected. If the same process as Example 1 is used, qualified magneto-optical glass cannot be produced. Therefore, the melting temperature and time are increased. At the same time, the range of transmittance higher than 70% is significantly reduced, and the maximum transmittance is significantly reduced.

[0062] Comparative Example 2

[0063] A high-transmittance magneto-optical glass comprises: 15 parts of Tb4O7, 0 parts of Dy2O3, 10 parts of Ga2O3, 45 parts of B2O3, 15 parts of SiO2, 6 parts of Na2O, and 4 parts of K2O; 0.15% of Sb2O3 is added to the above components.

[0064] The purity of the selected raw materials is above 99.99%, and the iron content of the raw materials is less than 5ppm.

[0065] The specific method for preparing glass includes the following steps:

[0066] Batching: Calculate the raw materials needed for the glass according to the glass composition, then weigh the raw materials and mix them evenly.

[0067] Melting: Place the mixture into a platinum crucible and place it into a silicon carbon rod electric furnace at 1280°C for 40 minutes.

[0068] Bubbling: After the glass is melted, high-purity dry oxygen is introduced into the glass for 30 minutes to fully melt the raw materials.

[0069] Clarification: Stop the oxygen supply, raise the temperature of the electric furnace to 1400℃, and carry out clarification to eliminate bubbles for 60 minutes.

[0070] Stirring and homogenizing: After clarification, the electric furnace is cooled to 1200°C, and a platinum stirrer is placed in the glass liquid for stirring. The stirring speed is 30r / min, and the stirring time is 30min. After stirring, let it stand for 15min.

[0071] Molding: Pour the glass liquid into the preheated mold quickly, and then quickly put the glass into the muffle furnace. Set the temperature of the muffle furnace to 650℃ and keep it warm for 10 minutes.

[0072] Annealing: anneal at a rate of 15°C / hour to 300°C, then cool to 80°C at 30°C / hour, close the muffle furnace and cool to room temperature.

[0073] The refractive index of the produced magneto-optical glass was tested, and the transmittance was less than 70% in the visible light and near-infrared wavelength range; the highest transmittance was 57.9% at a wavelength of 813nm.

[0074] Through Example 1 and Comparative Example 2: without adding Dy2O3, the transmittance of the magneto-optical glass is significantly reduced.

[0075] The principles, steps, etc. not explicitly described in the present invention are all obtainable by those skilled in the art through conventional technical means, and therefore will not be described in detail. Obviously, those skilled in the art can make various changes and modifications 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 equivalents, the present invention is also intended to include these modifications and variations.

Claims

1. A method for preparing magneto-optical glass with high transmittance, characterized in that: The glass composition is: 15 parts of Tb4O7, 5 parts of Dy2O3, 10 parts of Ga2O3, 45 parts of B2O3, 15 parts of SiO2, 6 parts of Na2O, 4 parts of K2O; 0.15 wt.% of Sb2O3 is added to the above components; or 21 parts of Tb4O7, 4 parts of Dy2O3, 10 parts of Ga2O3, 42 parts of B2O3, 14 parts of SiO2, 6 parts of Na2O, 3 parts of K2O; 0.15 wt.% of Sb2O3 is added to the above components; The method for preparing the magneto-optical glass with high transmittance comprises the following steps: a) Batching: Calculate the raw materials required for the glass according to the glass composition, then weigh the raw materials and mix them evenly; b) Melting: Place the mixture into a platinum crucible and place it into a silicon carbon rod electric furnace at 1200℃-1300℃ for 30-50min; c) Bubbling: After the glass is melted, high-purity dry oxygen is introduced into the glass for 20-30 minutes to fully melt the raw materials; d) Clarification: Stop the oxygen supply, raise the temperature of the electric furnace to 1400-1450℃, and perform clarification to eliminate bubbles for 60-90 minutes; e) Stirring and homogenizing: After clarification, cool the electric furnace to 1200-1250°C, place a platinum stirrer in the glass liquid for stirring, the stirring speed is 25-30r / min, the stirring time is 20-30min, and the stirring is completed and allowed to stand for 10-20min; f) Molding: Pour the glass liquid into the preheated mold quickly, and then quickly put the glass into the muffle furnace. Set the temperature of the muffle furnace to 650-700℃ and keep it warm for 10 minutes. g) Annealing: anneal at a rate of 15°C / hour to 300°C, then cool to 80°C at 30°C / hour, close the muffle furnace and cool to room temperature.

2. The method for preparing magneto-optical glass with high transmittance according to claim 1, characterized in that: The purity of the raw materials used is above 99.99%, and the iron content of the raw materials is less than 5ppm.

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