White jade glass-ceramics and method for preparing the same

Abstract

This application provides a white jade microcrystalline glass and its preparation method, belonging to the field of microcrystalline glass. The method involves mixing raw materials containing silicon, zirconium, rubidium, strontium, thorium, niobium, yttrium, and cadmium sources in a predetermined ratio to obtain a mixture; melting the mixture to form a glass melt; rolling the glass melt to obtain a glass strip of a predetermined thickness; annealing the glass strip; and then cooling and cutting it to obtain the white jade microcrystalline glass. This application, through unique component design and precise process control, successfully prepares an integrated material with a white jade-like texture and excellent physical properties, effectively solving the core technical problem of poor glass texture and lack of durability in traditional printing inks. By combining glass formation and white effect generation into one process, the production process is simplified, production efficiency is improved, and overall costs are reduced, meeting the requirements of high-end home appliances, architectural decoration, and other fields for long lifespan and high reliability of materials.

Description

Technical Field

[0001] This invention relates to the field of microcrystalline glass technology, specifically to a white jade microcrystalline glass and its preparation method. Background Technology

[0002] In the fields of modern home appliances, high-end architectural decoration, and consumer electronics, product appearance design has become a key factor determining market competitiveness. Consumers' growing demand for aesthetically pleasing, high-quality, and premium products has driven the development and application of new materials. Among these, white or jade-like glass substrates are highly favored by the market due to their simple and elegant characteristics.

[0003] Currently, the most common technical solution used in the industry to achieve a white effect on ordinary glass is surface printing. This process involves coating the glass surface with ink containing white pigments such as titanium dioxide through screen printing or inkjet printing, followed by high-temperature sintering and curing. However, this traditional technical approach has the following drawbacks: (1) Insufficient texture expression, as the white coating formed by the ink is a two-dimensional planar masking layer that cannot imitate the three-dimensional texture of natural white jade; (2) Shortcomings in physical properties and poor durability, as the ink coating and the glass substrate mainly rely on physical bonding rather than chemical fusion, making it susceptible to scratches, corrosion from cleaning agents, and environmental aging, leading to fading, scratches, and even peeling, thus affecting the service life; (3) Complex process, cumbersome procedures, and difficulty in controlling the yield rate, making it difficult to achieve advanced visual effects such as gradient, transparency, and layering.

[0004] In recent years, white jade microcrystalline glass, due to its high similarity in appearance and texture to natural jade, has seen increasing applications in refrigerator panels, air conditioner interiors, and high-end kitchen appliances, leading to rapid market demand growth. However, existing white jade microcrystalline glass or its preparation methods still suffer from high costs, complex processes, and unstable performance. Therefore, how to provide a microcrystalline glass with excellent performance, controllable cost, and the ability to stably achieve a white jade-like texture has become a pressing technical problem to be solved in this field.

[0005] In view of this, it is necessary to design a white jade microcrystalline glass and its preparation method to solve the above problems. Summary of the Invention

[0006] In view of the technical problems existing in the background art, this application provides a white jade microcrystalline glass and its preparation method, aiming to solve the technical problems of poor texture and unreliable performance of traditional white glass due to its reliance on surface coating.

[0007] In a first aspect, this application provides a method for preparing white jade microcrystalline glass, comprising the following steps: S1. Mix raw materials containing silicon source, zirconium source, rubidium source, strontium source, thorium source, niobium source, yttrium source and cadmium source in a predetermined ratio to obtain a mixture; S2. The mixture is melted to form molten glass; S3. The molten glass is rolled into a glass strip of a predetermined thickness; S4. Anneal the glass strip, and then cool and cut it to obtain white jade microcrystalline glass.

[0008] As a further improvement of this application, in step S1, the weight percentage of each component based on oxides is as follows: silicon dioxide 55~60%, zirconium dioxide 10~15%, rubidium oxide 7~11%, strontium oxide 4~6%, thorium dioxide 8~12%, niobium pentoxide 1~3%, yttrium oxide 1~3%, and cadmium oxide 1~3%.

[0009] As a further improvement of this application, in step S2, the melting treatment temperature is 1550~1600℃ and the time is 2~5h.

[0010] As a further improvement of this application, in step S3, the thickness of the glass strip is 2~5mm.

[0011] As a further improvement of this application, in step S4, the annealing process includes: heating the glass strip to 500~600℃, holding it at that temperature for 0.5~1.5h, and then slowly cooling it to below 200℃ at a cooling rate of 0.5~2℃ / min.

[0012] As a further improvement of this application, the D50 particle size of the raw material is 30~80μm.

[0013] Secondly, this application provides a white jade microcrystalline glass, which is prepared by the method for preparing white jade microcrystalline glass described in the first aspect.

[0014] As a further improvement of this application, the visible light transmittance of the white jade microcrystalline glass is 15-35%.

[0015] The beneficial effects of this application are as follows: This application provides a white jade microcrystalline glass and its preparation method. The method involves mixing raw materials containing silicon, zirconium, rubidium, strontium, thorium, niobium, yttrium, and cadmium sources in a predetermined ratio to obtain a mixture; melting the mixture to form a glass melt; rolling the glass melt to obtain a glass strip of a predetermined thickness; annealing the glass strip; and then cooling and cutting it to obtain the white jade microcrystalline glass. This application, through unique component design and precise process control, successfully prepares an integrated material with a white jade-like texture and excellent physical properties, effectively solving the core technical problem of poor glass texture and lack of durability in traditional printing inks.

[0016] This application introduces high-refractive-index oxides such as zirconium dioxide, thorium dioxide, and niobium pentoxide as core crystal phase forming agents, supplemented by rubidium oxide and strontium oxide as network exogenous oxides to regulate the glass structure, and uses yttrium oxide as a nucleating agent. Through synergistic effects, uniformly sized and diffusely distributed nano / submicron-sized grains are precipitated within the glass matrix. These grains form a significant refractive index difference with the glass matrix, producing a highly efficient volume scattering effect on visible light, rather than the surface masking of ink. This inside-out scattering endows the material with a warm, soft, and translucent jade-like texture. Simultaneously, by precisely controlling the component ratios, the visible light transmittance of the final product is maintained within the optimal range, perfectly replicating the hazy beauty and high-end feel of natural white jade.

[0017] The microcrystalline glass prepared in this application is a homogeneous material whose white effect originates from its internal crystalline structure rather than a surface physical coating. Therefore, it fundamentally avoids the problems common to ink coatings, such as scratches, peeling, fading, and poor chemical resistance. Its hardness, wear resistance, and chemical stability far exceed those of traditional printed glass, meeting the stringent requirements for long lifespan and high reliability in high-end home appliances, architectural decoration, and other fields.

[0018] The above description is only an overview of the technical solution of this application. In order to better understand the technical means of this application and to implement it in accordance with the contents of the specification, and to make the above and other objects, features and advantages of this application more obvious and understandable, the following are specific embodiments of this application. Attached Figure Description

[0019] To more clearly illustrate the technical solutions of this application, the accompanying drawings used in this application will be briefly described below. Obviously, the drawings described below are merely some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without any creative effort.

[0020] Figure 1 This is a physical image of the white jade microcrystalline glass provided in Embodiment 1 of this application. Detailed Implementation

[0021] The embodiments of the technical solution of this application will now be described in detail with reference to the accompanying drawings. These embodiments are only used to more clearly illustrate the technical solution of this application and are therefore merely examples, and should not be used to limit the scope of protection of this application.

[0022] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains; the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the application; the terms “comprising” and “having”, and any variations thereof, in the specification, claims, and foregoing description of the drawings are intended to cover non-exclusive inclusion.

[0023] In the description of the embodiments of this application, technical terms such as "first" and "second" are used only to distinguish different objects and should not be construed as indicating or implying relative importance or implicitly specifying the number, specific order, or primary and secondary relationship of the indicated technical features. In the description of the embodiments of this application, "multiple" means two or more, unless otherwise explicitly defined.

[0024] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.

[0025] In the description of the embodiments of this application, the term "multiple" refers to two or more (including two), similarly, "multiple sets" refers to two or more (including two sets), and "multiple pieces" refers to two or more (including two pieces).

[0026] In existing technologies, the most common methods for achieving white or decorative patterns on ordinary transparent or light-colored glass are screen printing or inkjet printing. These processes involve coating the glass surface with ink containing white pigment and then sintering it at high temperatures to cure it. However, this approach suffers from drawbacks such as poor finish and texture, insufficient durability and reliability, and complex and costly processes. Therefore, there is an urgent need for a new type of glass material that can achieve a seamless, jade-like texture without relying on surface coatings, while also possessing excellent durability and production efficiency.

[0027] To address the technical problems of poor texture and unreliable performance of traditional white glass due to its reliance on surface coatings, this application provides a white jade microcrystalline glass and its preparation method. In this method, uniformly sized and diffusely distributed nanoscale crystalline particles are induced to precipitate in the glass matrix as light scattering centers, thereby achieving a technical effect that makes the material exhibit a warm and smooth texture and semi-transparent effect resembling white jade from the inside out.

[0028] In a first aspect, embodiments of this application provide a method for preparing white jade microcrystalline glass, comprising the following steps: S1. Mix raw materials containing silicon source, zirconium source, rubidium source, strontium source, thorium source, niobium source, yttrium source and cadmium source in a predetermined ratio to obtain a mixture; S2. The mixture is melted to form molten glass; S3. Roll the molten glass to obtain a glass strip of a predetermined thickness; S4. Anneal the glass strip, then cool and cut it to obtain white jade microcrystalline glass.

[0029] In the technical solution of this application embodiment, the raw materials are mixed to ensure uniform distribution of each component. The mixture is melted at high temperature, and all solid raw materials undergo complex physicochemical reactions to form a single, uniform, and transparent glass melt. The high-temperature glass melt is then rapidly shaped into a glass strip of a predetermined thickness through rolling. The glass strip is heated to a specific temperature range for annealing, and then slowly cooled according to a strictly controlled cooling curve to eliminate internal thermal stress, improve its mechanical strength and stability, and make it less prone to breakage. Even after annealing, the glass strip is still at a relatively high temperature and needs further cooling to room temperature. Defects in the glass (such as bubbles, stones, scratches, unclear embossing, etc.) are then inspected. Finally, according to requirements, the glass strip is cut into sheets of specified dimensions using diamond tools. This application, through a complete process of raw material formulation design, melting to form a uniform glass melt, molding, and precision heat treatment to induce microcrystal precipitation, modifies the microstructure of the glass to closely resemble natural white jade, thus achieving a highly realistic effect in both visual and tactile aspects.

[0030] Furthermore, in some embodiments, in step S1, the weight percentage of each component based on oxides is as follows: silicon dioxide 55-60%, zirconium dioxide 10-15%, rubidium oxide 7-11%, strontium oxide 4-6%, thorium dioxide 8-12%, niobium pentoxide 1-3%, yttrium oxide 1-3%, and cadmium oxide 1-3%.

[0031] In the technical solution of this application embodiment, a carefully designed multi-component oxide formulation achieves efficient and controllable bulk crystallization in a glass matrix. Specifically, using silicon dioxide as a network framework, a powerful composite nucleating agent system is constructed using high contents of zirconium dioxide, thorium dioxide, and niobium pentoxide, inducing the formation of extremely high-density nanoscale nuclei during heat treatment. Subsequently, under the synergistic inhibition of yttrium trioxide and niobium pentoxide, the crystals grow uniformly into a submicron-scale structure. This dispersed microcrystalline phase causes strong light scattering, thereby endowing the material with a warm, milky-white jade-like texture. At the same time, rubidium oxide and strontium oxide regulate the melting process, while trace amounts of cadmium oxide are used to introduce a natural warm tone, ultimately constructing a microcrystalline glass composite material that combines the aesthetic appearance of white jade with excellent mechanical properties.

[0032] Furthermore, in some embodiments, in step S2, the melting temperature is 1550~1600℃ and the time is 2~5h.

[0033] In the technical solution of this application embodiment, the temperature and time of the melting treatment provide sufficient thermodynamic and kinetic conditions for the complex system containing multiple high-melting-point components. This high-temperature range ensures that all refractory oxides can be completely melted and fully dissolved in the silicate melt, while the sufficient holding time ensures that the melt achieves atomic-level uniform mixing through convection and diffusion, thereby eliminating compositional inhomogeneity and laying the foundation for the subsequent formation of uniformly distributed crystal nuclei and microcrystalline structures with consistent performance.

[0034] Furthermore, in some embodiments, in step S3, the thickness of the glass strip is 2~5mm.

[0035] In the technical solution of this application embodiment, the thickness range of the glass strip can ensure that the glass strip has sufficient heat capacity and mechanical strength during the rolling process, avoiding rapid cooling, breakage or deformation due to excessive thinness, and can also ensure that heat can be uniformly penetrated to the center of the glass strip during the subsequent annealing process, so as to achieve uniform crystallization from the surface to the interior, thereby obtaining a consistent jade-like texture.

[0036] Furthermore, in some embodiments, in step S4, the annealing process includes: heating the glass strip to 500~600°C, holding it at that temperature for 0.5~1.5h, and then slowly cooling it to below 200°C at a cooling rate of 0.5~2°C / min.

[0037] In the technical solution of this application embodiment, annealing helps to accurately release the internal stress of the glass and initially control the crystallization process. The temperature range of 500~600℃ is exactly near the transition temperature of the glass system. Holding at this temperature is sufficient to allow the atoms in the glass structure to release the internal stress generated by rolling and rapid cooling through short-range migration, preventing the glass from spontaneously cracking during subsequent processing or use. The subsequent extremely slow cooling rate is to minimize the generation of new and uncontrollable thermal stress due to excessive internal and external temperature differences when the glass passes through its brittle region, ensuring that the glass strip has excellent mechanical integrity and structural uniformity before entering the cutting process, providing a basic guarantee for finally obtaining a flawless, high-strength white jade microcrystalline glass product.

[0038] Furthermore, in some embodiments, the D50 particle size of the raw material is 30~80μm.

[0039] In the technical solution of this application embodiment, controlling the D50 particle size (i.e., median particle size) of the raw materials within a suitable range helps to optimize the efficiency and uniformity of the melting process. Smaller particles can accelerate the solid-phase reaction and melting rate, shorten the melting time and reduce energy consumption; at the same time, the particles are not too fine, thereby avoiding the adverse effects of agglomeration, moisture absorption, component segregation and flying caused by excessive specific surface area, ensuring the accuracy of batching and the uniformity of mixing.

[0040] Secondly, embodiments of this application provide a white jade microcrystalline glass, prepared by the method for preparing white jade microcrystalline glass described in the first aspect. The visible light (380~780nm) transmittance of this white jade microcrystalline glass is 15~35%.

[0041] In the technical solution of this application embodiment, through precise formula design and strict heat treatment process control, a large number of fine and uniformly distributed micron- or nano-sized crystals are precipitated in the glass matrix, thereby enabling the material to obtain a texture, luster and performance similar to white jade, which is suitable for high-end home appliances, building decoration and other fields.

[0042] The following are some specific embodiments. It should be noted that the embodiments described below are exemplary and are only used to explain this application, and should not be construed as limiting this application. Where specific techniques or conditions are not specified in the embodiments, they shall be performed in accordance with the techniques or conditions described in the literature in this field or according to the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be obtained commercially.

[0043] Example 1 This embodiment provides a method for preparing white jade microcrystalline glass, including the following steps: S1. Weigh and mix the raw materials precisely according to the following proportions by weight percentage: 58% silicon dioxide, 12% zirconium dioxide, 9% rubidium oxide, 5% strontium oxide, 10% thorium dioxide, 2% niobium pentoxide, 2% yttrium oxide, and 2% cadmium oxide to obtain a mixture; S2. The mixture is fed into a melting furnace and heated at a high temperature of 1580℃ to form a uniform, pure glass melt suitable for forming; S3. The molten glass flows out from the end of the furnace and enters a pair of rolling rollers. The high-temperature, viscous molten glass is continuously rolled between the rollers and rolled into a glass strip with a thickness of 3.2 mm under strong pressure. S4. The glass ribbon is placed in an annealing furnace and annealed at 550℃ for 1 hour. Then, it is slowly cooled to below 200℃ at a cooling rate of 1℃ / min. Afterward, it is further cooled to room temperature and cut to obtain white jade microcrystalline glass. Figure 1 As shown, qualified products are packaged and put into storage.

[0044] Example 2 This embodiment provides a method for preparing white jade microcrystalline glass. Compared with Example 1, the only difference is that the raw materials are: 55% silicon dioxide, 10% zirconium dioxide, 11% rubidium oxide, 6% strontium oxide, 12% thorium dioxide, 2% niobium pentoxide, 2% yttrium trioxide, and 2% cadmium oxide. Other experimental parameters and conditions are basically the same as in Example 1, and will not be repeated here.

[0045] Example 3 This embodiment provides a method for preparing white jade microcrystalline glass. Compared with Example 1, the only difference is that the raw materials are: 60% silicon dioxide, 15% zirconium dioxide, 7% rubidium oxide, 4% strontium oxide, 8% thorium dioxide, 2% niobium pentoxide, 2% yttrium trioxide, and 2% cadmium oxide. Other experimental parameters and conditions are basically the same as in Example 1, and will not be repeated here.

[0046] Example 4 This embodiment provides a method for preparing white jade microcrystalline glass. Compared with Example 1, the only difference is that the annealing temperature is 500℃ and held for 0.5h, and the cooling rate is 0.5℃ / min. Other experimental parameters and conditions are basically the same as those in Example 1, and will not be repeated here.

[0047] Example 5 This embodiment provides a method for preparing white jade microcrystalline glass. Compared with Example 1, the only difference is that the annealing temperature is 600℃ and held for 1.5h, and the cooling rate is 2℃ / min. Other experimental parameters and conditions are basically the same as those in Example 1, and will not be repeated here.

[0048] Comparative Example 1 Comparative Example 1 provides a method for preparing white jade microcrystalline glass. Compared with Example 1, the only difference is that the raw materials are: 65% silicon dioxide, 5% zirconium dioxide, 9% rubidium oxide, 5% strontium oxide, 10% thorium dioxide, 2% niobium pentoxide, 2% yttrium trioxide, and 2% cadmium oxide. Other experimental parameters and conditions are basically the same as those in Example 1, and will not be repeated here.

[0049] Comparative Example 2 Comparative Example 2 provides a method for preparing white jade microcrystalline glass. The only difference from Example 1 is that the raw materials are: 60% silicon dioxide, 15% zirconium dioxide, 0% rubidium oxide, 7% strontium oxide, 12% thorium dioxide, 3% niobium pentoxide, 3% yttrium trioxide, and 0% cadmium oxide. Other experimental parameters and conditions are basically the same as those in Example 1, and will not be repeated here.

[0050] Comparative Example 3 Comparative Example 3 provides a method for preparing white jade microcrystalline glass. Compared with Example 1, the only difference is that the melting temperature is 1450℃. Other experimental parameters and conditions are basically the same as those in Example 1, and will not be repeated here.

[0051] Comparative Example 4 Comparative Example 4 provides a method for preparing white jade microcrystalline glass. Compared with Example 1, the only difference is that the annealing temperature is 400℃. Other experimental parameters and conditions are basically the same as those in Example 1, and will not be repeated here.

[0052] The performance of the white jade microcrystalline glass obtained in the examples and comparative examples was tested, and the results are shown in Table 1.

[0053] Table 1. Performance test results of white jade microcrystalline glass obtained from the examples and comparative examples. "OK" means qualified, and "NG" means unqualified.

[0054] As can be seen from Table 1, this application effectively ensures the excellent performance and consistency of the white jade microcrystalline glass through unique component design and precise process control. In particular, under strict chemical testing (acid corrosion resistance test: 6 mol / L HCl solution, 6 h of boiling corrosion; alkali corrosion resistance test: equal volumes of 0.5 mol / L Na2CO3 solution and 1 mol / L NaOH solution mixed, 3 h of boiling corrosion), the surfaces of the samples in Examples 1-5 remained intact, indicating that the microcrystalline glass prepared in this application has excellent chemical stability and fully meets the durability requirements of high-end home appliances and building decoration. In Comparative Example 1, the excessive silica and insufficient zirconium dioxide levels resulted in an unstable glass structure and the presence of incompletely dissolved solid particles (stones) within the glass. Furthermore, the unbalanced formulation prevented the formation of an ideal microcrystalline structure, diminishing the jade-like texture of the material. In Comparative Example 2, the lack of rubidium oxide and cadmium oxide disrupted the synergistic effect of the formulation, leading to poor melt homogeneity, uncontrolled crystallization, and the inability to form effective light scattering centers. Consequently, the final product lost the warm, jade-like texture, resembling ordinary white glass or inferior ceramics in appearance. In Comparative Example 3, the excessively low melting temperature resulted in incomplete melting, poor homogenization of the molten glass, and the retention of numerous unmelted solid impurities (stones). Simultaneously, the gases in the molten glass could not escape smoothly, forming dense bubbles. In Comparative Example 4, the excessively low annealing temperature led to insufficient stress relief, causing microcracks or direct breakage of the glass with high internal stress during cooling and cutting.

[0055] It should be noted that this application is not limited to the above-described embodiments. The above embodiments are merely examples, and any embodiments with the same structure and effect as the technical concept within the scope of this application are included in the technical scope of this application. Furthermore, various modifications that can be conceived by those skilled in the art to the embodiments, and other ways of constructing by combining some of the constituent elements of the embodiments, without departing from the spirit of this application, are also included in the scope of this application.

Claims

1. A method for preparing white jade microcrystalline glass, characterized in that, Includes the following steps: S1. Raw materials containing silicon, zirconium, rubidium, strontium, thorium, niobium, yttrium, and cadmium sources are mixed in a predetermined ratio to obtain a mixture; the weight percentage of each component based on oxides is as follows: silicon dioxide 55-60%, zirconium dioxide 10-15%, rubidium oxide 7-11%, strontium oxide 4-6%, thorium dioxide 8-12%, niobium pentoxide 1-3%, yttrium trioxide 1-3%, and cadmium oxide 1-3%; S2. The mixture is melted to form molten glass; S3. The molten glass is rolled into a glass strip of a predetermined thickness; S4. Anneal the glass strip, and then cool and cut it to obtain white jade microcrystalline glass.

2. The method for preparing white jade microcrystalline glass according to claim 1, characterized in that, In step S2, the melting treatment temperature is 1550~1600℃ and the time is 2~5h.

3. The method for preparing white jade microcrystalline glass according to claim 1, characterized in that, In step S3, the thickness of the glass strip is 2~5mm.

4. The method for preparing white jade microcrystalline glass according to claim 1, characterized in that, In step S4, the annealing process includes: heating the glass strip to 500~600℃, holding it at that temperature for 0.5~1.5h, and then slowly cooling it to below 200℃ at a cooling rate of 0.5~2℃ / min.

5. The method for preparing white jade microcrystalline glass according to claim 1, characterized in that, The D50 particle size of the raw material is 30~80μm.

6. A type of white jade microcrystalline glass, characterized in that, It is prepared by the method of any one of claims 1-5 for preparing white jade microcrystalline glass.

7. The white jade microcrystalline glass according to claim 6, characterized in that, The visible light transmittance of the white jade microcrystalline glass is 15-35%.

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