Method for preparing oxide glass based on induction melting process and oxide glass

By using composite crucibles and electromagnetic induction heating technology, the problems of large-scale production, pollution, and atmosphere control in oxide glass preparation have been solved, enabling the efficient and low-cost preparation of large-size, high-purity oxide glass.

CN121850319APending Publication Date: 2026-04-14UNIV OF SCI & TECH BEIJING
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
UNIV OF SCI & TECH BEIJING
Filing Date
2026-01-06
Publication Date
2026-04-14

AI Technical Summary

Technical Problem

Existing technologies make it difficult to achieve large-scale production in oxide glass preparation. Traditional tank furnace melting methods suffer from high energy consumption, long cycles, and crucible material contamination. Electromagnetic induction melting, on the other hand, faces challenges such as unsuitable atmospheric conditions and changes in glass composition.

Method used

A composite crucible structure is adopted, including a first oxide layer, a conductive material layer, and a second oxide layer, with a protective felt sandwiched between them. Combined with electromagnetic induction heating, rapid melting and precise temperature control of oxide glass are achieved through staged power control and atmosphere adjustment.

Benefits of technology

This technology enables the efficient preparation of large-size oxide glasses, reduces carburization and ion migration contamination, lowers production costs, and ensures the high purity and excellent performance of the glass.

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Abstract

The invention discloses a method for preparing oxide glass based on an induction melting process and the oxide glass, the preparation method comprises the following steps: using a composite crucible to bear initial glass powder, the composite crucible comprises a first oxide layer, a conductive material layer and a second oxide layer which are arranged from outside to inside, a gap is formed between the second oxide layer and the conductive material layer, the composite crucible further comprises a protective felt, the gap is filled with the protective felt, the protective felt wraps the outer side of the second oxide layer, the protective felt is of a fiber structure, and the melting point of the protective felt is not lower than that of the initial glass powder; the initial glass powder is heated to a molten state through electromagnetic induction, a melt is obtained, the heating power in the first stage is in positive correlation with the heating time, and the heating power in the second stage is in a decreasing trend; and carrying out casting molding on the melt, and cooling to obtain the oxide glass.
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Description

Technical Field

[0001] This invention relates to the field of oxide glass materials technology, and in particular to a method for preparing oxide glass based on induction melting process and oxide glass. Background Technology

[0002] Currently, high-entropy oxide glasses have attracted widespread attention and have already seen initial applications in some fields due to their excellent mechanical and optical properties. However, these materials typically have high melting points, and existing preparation processes mainly rely on containerless solidification, which can only produce small-sized samples and is difficult to scale up for production. Traditional tank furnace melting methods are limited by the upper limit of operating temperature and suffer from problems such as long preparation cycles and high energy costs.

[0003] Electromagnetic induction melting boasts significant advantages such as rapid heating, high thermal efficiency, and low energy consumption, making it commonly used in metal smelting. However, its direct application in the preparation of oxide glasses faces two major challenges: first, the compatibility between commonly used crucible materials and molten glass can easily lead to contamination; second, existing process atmospheres are unsuitable for oxide systems, potentially causing changes in glass composition or performance degradation. These issues severely restrict the application of this method in the preparation of high-quality oxide glasses.

[0004] Therefore, it is necessary to develop a method for preparing oxide glass based on electromagnetic induction melting. By solving core issues such as crucible compatibility and process atmosphere control, this method can leverage the high efficiency and energy-saving advantages of induction melting while ensuring the high purity and excellent performance of the glass products. Summary of the Invention

[0005] The present invention aims to solve one of the technical problems in related technologies to a certain extent, and provides a method for preparing oxide glass based on induction melting process and oxide glass.

[0006] As a first aspect of the present invention, a method for preparing oxide glass based on an induction melting process is provided, the preparation method comprising: An initial glass powder is supported by a composite crucible. The composite crucible includes a first oxide layer, a conductive material layer, and a second oxide layer arranged from the outside to the inside. There is a gap between the second oxide layer and the conductive material layer. The composite crucible also includes a protective felt, which is filled in the gap and wrapped around the outside of the second oxide layer. The protective felt has a fibrous structure and the melting point of the protective felt is not lower than the melting point of the initial glass powder. The initial glass powder is heated to a molten state using electromagnetic induction to obtain a melt. In the first stage, the heating power is positively correlated with the heating time, while in the second stage, the heating power shows a decreasing trend. The molten material is cast and cooled to obtain the oxide glass.

[0007] Further, heating the initial glass powder to a molten state using electromagnetic induction includes: The composite crucible is heated to a set temperature in the first stage using a coil. The heating power of the coil is positively correlated with the heating time. The composite crucible also includes a connecting felt, which is disposed on the outside of the first oxide layer. The coil is sleeved on the outside of the composite crucible and fixedly connected to the first oxide layer through the connecting felt. The composite crucible is kept at a constant temperature during the second stage, during which the heating power of the coil is reduced.

[0008] Furthermore, the set temperature is between 1000℃ and 2200℃, and the heating rate is between 1℃ / min and 50℃ / min.

[0009] Furthermore, in the step of heating the composite crucible to a set temperature in the first stage using a coil, the process gas used includes at least one of oxygen, air, argon, and nitrogen.

[0010] Furthermore, the protective felt includes at least one of alumina felt, graphite felt, mullite felt, and aluminum silicate felt.

[0011] Furthermore, the material of the first oxide layer includes quartz, the material of the conductive material layer includes at least one of graphite, tantalum, tungsten and molybdenum, and the material of the second oxide protective layer includes at least one of alumina, zirconium oxide, magnesium oxide and ceramics.

[0012] Furthermore, the initial glass powder includes SiO2, B2O3, Na2O, Li2O, Al2O3, CaO, ZnO, BaO, TiO2, ZrO2, Y2O3, Gd2O3, La2O3, Ta2O5, and Nd2O3.

[0013] Further, the molten material is cast and cooled to obtain the oxide glass, comprising: Provide preheated molds; The molten material is poured into the preheated mold to obtain a first glass sample; The glass intermediate was subjected to heat preservation annealing treatment to obtain a second glass sample; The second glass sample was cooled in the furnace and then removed to obtain the oxide glass.

[0014] Furthermore, in the step of heat preservation and annealing the glass intermediate, the annealing temperature is between 200°C and 700°C, and the heat preservation time is between 0.5h and 4h.

[0015] As a second aspect of this application, an oxide glass is provided, which is prepared by the above-described preparation method.

[0016] Compared with existing technologies, the beneficial technical effects of this invention lie in the successful introduction of highly efficient, ultra-high temperature electromagnetic induction melting technology into the field of oxide glass preparation, developing a novel glass preparation process based on this technology. This method addresses the complex compositional system and thermal properties of oxide glasses by developing and designing a specific composite crucible. The nested three protective layers and the sandwiched protective felt effectively avoid carburization and ion migration problems caused by induction melting, reducing glass contamination. Simultaneously, considering the thermodynamic characteristics of oxide glasses during the heating process, new heating parameters are specifically adopted to achieve rapid heating of the oxide glass while enabling more precise temperature control, reducing overheating or underheating problems. The oxide glass prepared using the method of this application has fewer defects, a purer appearance, and is suitable for large-size mass production, significantly reducing production costs.

[0017] These features and advantages of the present invention will be disclosed in detail in the following specific embodiments and accompanying drawings. The preferred embodiments or means of the present invention will be shown in detail in conjunction with the accompanying drawings, but are not intended to limit the technical solutions of the present invention. In addition, each of these features, elements and components appearing in the following text and drawings is a plurality of, and different symbols or numbers are used for convenience of representation, but all represent parts with the same or similar construction or function. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.

[0019] Figure 1 This is a flowchart of one embodiment of the method for preparing oxide glass provided by the present invention; Figure 2(a) is a time-temperature relationship diagram of one embodiment of the electromagnetic induction heating oxide glass provided by the present invention; Figure 2(b) is a time-heating power relationship diagram of one embodiment of the electromagnetic induction heating oxide glass provided by the present invention; Figure 3 A schematic diagram illustrating one embodiment of the method for preparing oxide glass provided by the present invention; Figure 4This is a photograph of a glass sample prepared by induction melting technology according to Embodiment 1 of the present invention. Figure 5 The XRD patterns of the glass samples prepared by induction melting technology provided in Examples 1 to 3 of this invention; Figure 6(a) is a photograph of the protective felt after the composite crucible was used to prepare oxide glass in Example 1 of the present invention. Figure 6(b) is a photograph of the bottom of the crucible after oxide glass preparation using the composite crucible in Example 1 of this invention. Figure 7(a) is a photograph of the protective felt after the composite crucible was used to prepare oxide glass in Comparative Example 1 of the present invention. Figure 7(b) is a photograph of the bottom of the crucible after oxide glass was prepared using the composite crucible in Comparative Example 1 of the present invention. Figure 7(c) is a photograph of the appearance of the oxide glass prepared by the composite crucible in Comparative Example 1 of the present invention. Detailed Implementation

[0020] Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described are intended to explain the present invention and should not be construed as limiting the invention.

[0021] The terms "an embodiment," "example," or "trademark" used in this specification refer to a particular feature, structure, or characteristic described in connection with the embodiment itself that may be included in at least one embodiment disclosed in this invention. The phrase "in an embodiment" appearing in various places throughout the specification does not necessarily refer to the same embodiment.

[0022] Cover glass, as an essential outer protective component for electronic devices, plays a vital role in protecting them. With the increasingly diverse applications of electronic devices, more stringent standards are being set for the drop resistance and scratch resistance of cover glass. The intrinsic hardness and Young's modulus of the glass are key factors determining these properties.

[0023] Glass is a high-performance inorganic non-metallic material and one of the country's important pillar industries. Its application has a long history, dating back to the Middle East around 2500 BC. Over the centuries, the glass industry has evolved from intermittent crucible furnaces to continuous tank furnaces, significantly increasing production capacity.

[0024] The inventors of this application have discovered that while traditional tank furnace melting can achieve continuous production in industrial manufacturing, it faces significant bottlenecks when dealing with small-batch, multi-variety special glass orders (such as rare-earth-doped laser glass). Each formula change requires emptying the tank furnace and reheating, leading to complex start-up and adjustment processes and significantly increasing the time cost and energy consumption per unit product. For glass samples requiring rapid performance verification (such as radiation-resistant glass for aerospace applications), this inefficiency can delay project progress and hinder the application and promotion of new materials. Furthermore, the key components used in traditional processes are mostly platinum-rhodium alloys, whose melting point limits the maximum operating temperature to 1650-1700℃, which also restricts the range of glass compositions that can be produced.

[0025] During the glass R&D stage, frequent changes in formulations and diversified demands further highlight the inadequacy of traditional tank furnaces. Traditional lifting melting furnaces also have significant limitations: the preparation cycle is long, typically requiring 1-2 days for a single sample, and multiple comparative experiments exponentially increase the time required. Furthermore, limited by the crucible and furnace structure, their maximum heating temperature can only reach 1650-1700℃, failing to meet the requirements for preparing high-melting-point glasses, thus restricting the selection of glass material composition and performance development. In recent years, however, some specialized ultra-high temperature preparation methods have been widely applied in glass R&D. For example, CN108929034A discloses a method for preparing lanthanum titanate-based glass sheets using a laser-heated pneumatic suspension device based on containerless solidification technology, and CN101948249A discloses a method for preparing high-refractive-index microsphere glass using a flame jet method, etc. While these methods can produce glass samples in a short time, with temperatures far exceeding 1700℃ and even reaching 3000℃ in a short period, the sample sizes are limited to millimeters (e.g., containerless solidified glass is at most 8mm), or even powder (e.g., glass prepared by flame jetting is mostly micron-sized powder), making it difficult to meet practical application needs. Overall, existing glass preparation processes can no longer keep pace with the research and development and production of new glass materials.

[0026] Introducing vacuum induction melting technology—a core process in metallurgy—into glass manufacturing is expected to effectively solve the aforementioned problems of inefficiency and limited melting temperature. Its core principle is that under the influence of a high-frequency alternating magnetic field, a high-density circular current is induced within a conductive material (or a specialized crucible), generating a concentrated and intense thermal effect that rapidly melts the material. This is further enhanced by a high-vacuum environment (vacuum degree up to 10⁻⁵). -3 -10 -5 This technology (Pa) enables efficient degassing, impurity removal, and precise composition control. Its significant advantages include high heating efficiency, fast speed, low energy consumption, and environmental friendliness. It utilizes the conductive material's own induction heating under a high vacuum / semi-vacuum inert atmosphere, or employs a graphite crucible for induction heating, achieving a maximum operating temperature of 2200℃.

[0027] However, applying this technology to glassmaking faces the following key challenges. First, there's the issue of crucible compatibility: traditional glassmaking typically uses oxide or platinum crucibles in a neutral / weakly oxidizing atmosphere. Furthermore, the glass raw material powder itself is not conductive; when using vacuum induction melting, a conductive crucible is required as the heating source. If graphite or metal crucibles (such as tungsten, molybdenum, or tantalum) commonly used in vacuum induction melting are used, there is a risk of graphite carburization or metal contamination, severely affecting glass formation. Second, there's the issue of atmosphere conflict: vacuum induction melting usually requires a high vacuum / inert or reducing atmosphere to protect the graphite or metal crucible. Oxide glass melting, however, is typically carried out in an air / oxygen atmosphere. Under a reducing atmosphere, the valence states of key elements in the glass (especially multivalent elements) may become uncontrolled, leading to performance degradation and color development problems.

[0028] Therefore, in summary, the core of this invention lies in: by innovatively solving the problems of crucible compatibility and atmosphere control, successfully introducing efficient and high-temperature induction melting technology into the field of glass preparation, and developing a new glass preparation method based on this technology.

[0029] As a first aspect of the present invention, a method for preparing oxide glass based on an induction melting process is provided, such as... Figure 1 and Figure 3 As shown, the preparation method includes: S100. Using a composite crucible to hold initial glass powder, the composite crucible includes a first oxide layer, a conductive material layer and a second oxide layer arranged from the outside to the inside, with a gap between the second oxide layer and the conductive material layer, the composite crucible also includes a protective felt, the protective felt is filled in the gap and wrapped around the outside of the second oxide layer, the protective felt has a fibrous structure, and the melting point of the protective felt is not lower than the melting point of the initial glass powder. S200. Electromagnetic induction is used to heat the initial glass powder to a molten state to obtain a melt. In the first stage, the heating power is positively correlated with the heating time, and in the second stage, the heating power shows a decreasing trend. S300: The molten material is cast and cooled to obtain oxide glass.

[0030] Compared with existing technologies, the beneficial technical effects of this invention lie in the successful introduction of highly efficient, ultra-high temperature electromagnetic induction melting technology into the field of oxide glass preparation, developing a novel glass preparation process based on this technology. This method addresses the complex compositional system and thermal properties of oxide glasses by developing and designing a specific composite crucible. The nested three protective layers and the sandwiched protective felt effectively avoid carburization and ion migration problems caused by induction melting, reducing glass contamination. Simultaneously, considering the thermodynamic characteristics of oxide glasses during the heating process, new heating parameters are specifically adopted to achieve rapid heating of the oxide glass while enabling more precise temperature control, reducing overheating or underheating problems. The oxide glass prepared using the method of this application has fewer defects, a purer appearance, and is suitable for large-size mass production, significantly reducing production costs.

[0031] In step S100, this application does not impose any special limitations on the composition of the initial glass powder, as long as it is an oxide glass composition. Preferably, the initial glass powder includes SiO2, B2O3, Na2O, Li2O, Al2O3, CaO, ZnO, BaO, TiO2, ZrO2, Y2O3, Gd2O3, La2O3, Ta2O5, and Nd2O3.

[0032] This application does not impose any special limitations on the specific composition of the composite crucible, as long as it meets the temperature required for induction melting. In some embodiments, the material of the first oxide layer includes quartz, the material of the conductive material layer includes at least one of graphite, tantalum, tungsten and molybdenum, and the material of the second oxide protective layer includes at least one of alumina, zirconium oxide, magnesium oxide and ceramics.

[0033] This application does not impose any special limitations on how the composite crucible is formed into a composite structure. For example, it can be formed by applying multiple layers of coating, or by using a nested crucible structure. Preferably, a nested crucible structure is used, such as... Figure 3 As shown, the outermost layer uses a quartz crucible (i.e., a protective crucible). The quartz crucible can isolate the induction coil from the high-temperature heat source, avoiding electromagnetic interference and metal vapor corrosion. The middle layer uses a graphite crucible (i.e., a conductive crucible) as the heat source for induction heating. The quartz crucible is used as a protective crucible in combination with the conductive graphite crucible. The innermost layer can use an oxide crucible, such as an alumina crucible, a zirconia crucible, a magnesium oxide crucible, or a ceramic crucible, which has higher chemical stability and avoids reaction with glass components at high temperatures or contamination of the glass.

[0034] To prevent the graphite crucible from seeping into the glass material at high temperatures and causing contamination, this application also includes a protective felt, such as... Figure 3The high-temperature resistant felt shown uses a loose fibrous structure in the middle to block carburization. This application does not specifically limit the composition of the protective felt, as long as it can isolate carburization and withstand high temperatures and conduct heat. Preferably, the protective felt includes at least one of alumina felt, graphite felt, mullite felt, and aluminosilicate felt. Simultaneously, the protective felt of this application can serve as a filler between each layer of crucibles. Depending on the required temperature and crucible type, the high-temperature resistant felt is used to wrap and position each layer of crucibles. To fully isolate carburization, preferably, the protective felt of this application completely wraps around the crucible.

[0035] In step S200, as an optional implementation, electromagnetic induction is used to heat the initial glass powder to a molten state, including: The composite crucible is heated to a set temperature in the first stage using a coil. The heating power of the coil is positively correlated with the heating time. The composite crucible also includes a connecting felt, which is disposed on the outside of the first oxide layer. The coil is sleeved on the outside of the composite crucible and fixedly connected to the first oxide layer through the connecting felt. The composite crucible is kept at a constant temperature during the second stage, during which the heating power of the coil is reduced.

[0036] It is worth noting that this application does not simply adjust the power for heating arbitrarily. While higher power generally results in faster heating, the heating process of oxides involves complex chemical mixing reactions, generating additional endothermic or exothermic reactions, making it more difficult to control the electromagnetic induction temperature. This is especially true for indirect temperature control via coil power; unsuitable temperatures and heating rates can produce undesirable byproducts. For example, excessively fast heating, particularly with volatile or decomposable oxides, can easily cause "smoke." Excessive smoke affects the observation of the oxide heating stage and severely interferes with infrared thermography, making accurate temperature detection impossible. Conversely, excessively slow heating or prolonged heating leads to excessive volatilization in the middle graphite crucible, and the innermost crucible is difficult to use at high temperatures for extended periods. This application develops electromagnetic induction heating process parameters for oxide glass components through a combination of complex theoretical derivation and extensive experimental verification. In a specific embodiment, this application controls the temperature to achieve a stable rise and holding stage by adjusting the heating power in stages, as shown in Figures 2(a) and 2(b). Preferably, the heating power is between 1kW and 8kW. Using the power control curve shown in Figure 2, a stable melting temperature can be obtained at the maximum power. After reaching the set melting temperature, it is necessary to ensure that the temperature is kept stable for a period of time to provide a stable melting reaction environment. At this time, the power is kept at the maximum power for a period of time and then slowly reduced. The temperature can drop slightly within an acceptable range, thereby achieving the heat preservation effect. Furthermore, the slow drop in temperature is beneficial to the subsequent cooling and casting.

[0037] Preferably, the set temperature is between 1000℃ and 2200℃, and the heating rate is between 1℃ / min and 50℃ / min.

[0038] In the step of heating the composite crucible to a set temperature using a coil in the first stage, the process gas used includes at least one of oxygen, air, argon, and nitrogen. In conventional metal smelting, because metals oxidize in air, the process is carried out in an inert atmosphere, which is detrimental to the melting of oxide glasses. This application uses a quartz crucible, a graphite crucible, and an inner oxide crucible to suppress oxidation in an air atmosphere.

[0039] In step S300, as an optional implementation, the molten material is cast and cooled to obtain oxide glass, comprising: Provide preheated molds; The molten material is poured into a preheated mold to obtain the first glass sample; The glass intermediate was subjected to heat preservation and annealing treatment to obtain the second glass sample; The second glass sample was removed after cooling in the furnace, yielding oxide glass.

[0040] Preferably, in the step of heat preservation and annealing the intermediate glass product, the annealing temperature is between 200°C and 700°C, and the heat preservation time is between 0.5h and 4h.

[0041] As a second aspect of this application, an oxide glass is provided, which is prepared by the above-described preparation method.

[0042] Compared with existing technologies, the beneficial technical effects of this invention lie in the successful introduction of highly efficient, ultra-high temperature induction melting technology into the field of glass preparation, and the development of a novel glass preparation process based on this technology. This method can achieve rapid heating, reaching a crucible temperature of 2200℃ in as little as 0.5 hours, and can prepare glass samples with dimensions larger than centimeters. Addressing the issues of carburization in graphite crucibles and ion migration in metal crucibles that can contaminate the molten glass, this invention designs a composite crucible system that effectively blocks contamination from conductive crucibles, thereby ensuring the purity of the glass samples.

[0043] The present invention will be further illustrated below through specific embodiments.

[0044] Example Example 1 This invention provides a method for preparing soda-lime silica glass based on induction melting process, the steps of which are as follows: S1. Mix powdered SiO2, Al2O3, CaO, MgO, Na2O, and (NH4)2SO4 in a molar ratio of 70%:1%:8.5%:4%:15%:1.5% to obtain glass raw material; S2. Use a quartz crucible as a protective crucible, a graphite crucible as a conductive crucible, and a magnesium oxide crucible as an oxide crucible. Use alumina felt as a filler to combine the three crucibles and fix them on the induction coil. Add the glass raw material described in S1 into the innermost crucible. S3. Use air atmosphere, no vacuuming is required, just keep the air inlet open; S4. Heating: The crucible temperature is controlled by controlling the coil current. The temperature is rapidly increased to 1650℃ in 1.2 hours to obtain glass melt. The melt is then stirred multiple times to ensure it is fully melted. S5. After holding at 1650℃ for 2 hours, the glass is cast and annealed in a mold preheated to 500℃ for 3 hours to eliminate the internal stress generated during the cooling process, and finally transparent glass is obtained.

[0045] like Figure 4As shown, the prepared glass is free from carburization, metal contamination, and other obvious defects. Furthermore, the prepared glass maintains a well-defined amorphous structure.

[0046] Example 2 This invention provides a method for preparing borosilicate glass based on induction melting process, the steps of which are as follows: S1. Mix powdered SiO2, Al2O3, B2O3, CaO, MgO, SnO2, and (NH4)2SO4 in a molar ratio of 50%:10%:25%:8%:4%:1%:2% to obtain glass raw material; S2. Use a quartz crucible as a protective crucible, a graphite crucible as a conductive crucible, and an alumina crucible as an oxide crucible. Combine the three crucibles with mullite felt as a filler and fix them on the induction coil. Add the glass raw material described in S1 into the innermost crucible. S3. Use air atmosphere, no vacuuming is required, just keep the air inlet open; S4. Heating: The crucible temperature is controlled by controlling the coil current. The temperature is rapidly increased to 1450℃ in 1 hour to obtain glass melt. The melt is then stirred multiple times to ensure it is fully melted. S5. After holding at 1450℃ for 3 hours, the glass is cast and annealed in a mold preheated to 300℃ for 2 hours to obtain transparent glass.

[0047] Example 3 This invention provides a method for preparing high-melting-point, high-entropy oxide glass based on induction melting process, the steps of which are as follows: S1. Mix TiO2, ZrO2, Y2O3, Al2O3, La2O3, SiO2, B2O3, and (NH4)2SO4 in a molar ratio of 20%:10%:4%:30%:15%:10%:10%:1% to obtain glass raw material; S2. Use a quartz crucible as a protective crucible, a graphite crucible as a conductive crucible, and a zirconium oxide crucible as an oxide crucible. Combine the three crucibles with aluminum silicate felt as a filler and fix them on the induction coil. Add the glass raw material described in S1 into the innermost crucible. S3. Use air atmosphere, no vacuuming is required, just keep the air inlet open; S4. Heating: The crucible temperature is controlled by controlling the coil current. The temperature is rapidly increased to 1800℃ in 1.5 hours to obtain glass melt. The melt is then stirred multiple times to ensure it is fully melted. S5. After holding at 1800℃ for 1.5 hours, the glass is cast and annealed in a mold preheated to 700℃ for 4 hours to obtain transparent glass.

[0048] Example 4 This invention provides a method for preparing high-melting-point oxide glass based on induction melting process, the steps of which are as follows: S1. High-purity quartz (purity greater than 99.95%) is used as the glass raw material; S2. Use a quartz crucible as a protective crucible, a graphite crucible as a conductive crucible, and a zirconium oxide crucible as an oxide crucible. Combine the three crucibles with mullite felt as a filler and fix them on the induction coil. Add the glass raw material described in S1 into the innermost crucible. S3. Use air atmosphere, no vacuuming is required, just keep the air inlet open; S4. Heating: The crucible temperature is controlled by controlling the coil current. The temperature is rapidly increased to 2100℃ in 2 hours to obtain glass melt. The melt is then stirred multiple times to ensure it is fully melted. S5. After holding at 2100℃ for 1 hour, the glass is cast and annealed in a mold preheated to 700℃ for 4 hours to obtain transparent glass.

[0049] Comparative Example Comparative Example 1 Oxide glass was prepared using the same preparation method as in Example 1, except that the crucible was not completely wrapped with alumina felt.

[0050] Test case The structures of the oxide glasses in Examples 1 to 3 were characterized using a Smartlab 9 X-ray diffractometer from Japan Co., Ltd., as follows: Figure 5 As shown, the XRD pattern exhibits the broad diffraction peaks characteristic of amorphous materials, indicating that the prepared sample is indeed an amorphous glass.

[0051] This invention, based on induction melting technology, develops an integrated platform capable of glass melting, shaping, and annealing under various atmospheres. This novel glass preparation technology enables rapid heating and precise, stable temperature control, efficiently completing glass melting and preparation, supporting the preparation of large-size samples, and significantly improving experimental efficiency.

[0052] The crucibles of Example 1 and Comparative Example 1 were photographed, as shown in Figures 6(a), 6(b), 7(a), and 7(b). It can be seen that the alumina felt in Figures 6(a) and 6(b) has good coverage of the crucible, and after firing, carburization basically did not occur, and the inside of the crucible is transparent and colorless. It can be seen from Figures 7(a) and 7(b) that the alumina felt that does not completely cover the crucible produces obvious carburization, and carburization has occurred to the inner layer of the crucible, and the inside of the crucible is grayish-brown. Figure 7(c) shows the glass contaminated by carburization.

[0053] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing oxide glass based on induction melting process, characterized in that, Preparation methods include: An initial glass powder is supported by a composite crucible. The composite crucible includes a first oxide layer, a conductive material layer, and a second oxide layer arranged from the outside to the inside. There is a gap between the second oxide layer and the conductive material layer. The composite crucible also includes a protective felt, which is filled in the gap and wrapped around the outside of the second oxide layer. The protective felt has a fibrous structure and the melting point of the protective felt is not lower than the melting point of the initial glass powder. The initial glass powder is heated to a molten state using electromagnetic induction to obtain a melt. In the first stage, the heating power is positively correlated with the heating time, while in the second stage, the heating power shows a decreasing trend. The molten material is cast and cooled to obtain the oxide glass.

2. The preparation method according to claim 1, characterized in that, Heating the initial glass powder to a molten state using electromagnetic induction includes: The composite crucible is heated to a set temperature in the first stage using a coil. The heating power of the coil is positively correlated with the heating time. The composite crucible also includes a connecting felt, which is disposed on the outside of the first oxide layer. The coil is sleeved on the outside of the composite crucible and fixedly connected to the first oxide layer through the connecting felt. The composite crucible is kept at a constant temperature during the second stage, during which the heating power of the coil is reduced.

3. The preparation method according to claim 2, characterized in that, The set temperature is between 1000℃ and 2200℃, and the heating rate is between 1℃ / min and 50℃ / min.

4. The preparation method according to claim 2, characterized in that, In the step of heating the composite crucible to a set temperature in the first stage using a coil, the process gas used includes at least one of oxygen, air, argon, and nitrogen.

5. The preparation method according to claim 1, characterized in that, The protective felt includes at least one of alumina felt, graphite felt, mullite felt, and aluminum silicate felt.

6. The preparation method according to claim 1, characterized in that, The first oxide layer is made of quartz, the conductive material layer is made of at least one of graphite, tantalum, tungsten and molybdenum, and the second oxide protective layer is made of at least one of alumina, zirconium oxide, magnesium oxide and ceramics.

7. The preparation method according to any one of claims 1 to 6, characterized in that, The initial glass powder includes SiO2, B2O3, Na2O, Li2O, Al2O3, CaO, ZnO, BaO, TiO2, ZrO2, Y2O3, Gd2O3, La2O3, Ta2O5, and Nd2O3.

8. The preparation method according to any one of claims 1 to 6, characterized in that, The molten material is cast and cooled to obtain the oxide glass, comprising: Provide preheated molds; The molten material is poured into the preheated mold to obtain a first glass sample; The glass intermediate was subjected to heat preservation annealing treatment to obtain a second glass sample; The second glass sample was cooled in the furnace and then removed to obtain the oxide glass.

9. The preparation method according to claim 8, characterized in that, In the step of heat preservation and annealing the glass intermediate, the annealing temperature is between 200°C and 700°C, and the heat preservation time is between 0.5h and 4h.

10. An oxide glass, characterized in that, The oxide glass is prepared by the preparation method described in any one of claims 1 to 9.

Citation Information

Patent Citations

  • Environmental-friendly microsphere glass with high refractive index and preparation method thereof

    CN101948249A

  • Lanthanum titanate-based glass sheet as well as preparation method and application of lanthanum titanate-based glass sheet

    CN108929034A