Method for firing bead point granular frosted glaze
By precisely controlling the firing process and raw material formula, combined with glaze spraying technology and electric kiln firing, a uniform bead-dot granular glaze surface is formed, which solves the problem of inaccurate morphology and distribution of glaze surface particles in the existing technology, and achieves high-quality, beautiful and easy-to-clean ceramic products.
Patent Information
- Application Number
- CN202510396259.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-31
- Publication Date
- 2025-06-24
AI Technical Summary
The existing ceramic glaze firing process is difficult to achieve precise control of the morphology and distribution of glaze particles, resulting in unstable product quality and poor appearance effects, and neglecting the cleaning problem of glaze in actual use.
By precisely controlling the firing process and raw material formula, glazes of SiO2, Al2O3, K2O, Na2O and component A (including TiO2 and B2O3) are used to ball mill and adjust the moisture content of the glaze water. Combined with glaze spraying technology and electric kiln firing, a uniform bead-point granular glaze surface is formed.
It realizes precise control of the glaze particle size, forms a unique and beautiful texture, has good light transmission and easy cleaning characteristics, and meets the needs of high-quality, beautiful and practical ceramic products.
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of ceramic firing, and specifically relates to a firing method for a bead-like granular frosted glaze surface. Background Art
[0002] In the current field of ceramic product production, consumers have put forward higher and higher requirements for the aesthetics and practicality of ceramic products. With the improvement of living standards, while people pursue the artistic value of ceramic products, they also pay more attention to the convenience of daily use and the simplicity of cleaning. Precise control of the size, shape, and distribution of glaze particles is such that glaze defects are not likely to occur during the firing process, resulting in unstable product quality. It can meet the market demand for high-quality, beautiful, and easy-to-clean ceramic products. However, traditional ceramic glaze firing processes often can only provide relatively single surface effects, such as smooth glaze surfaces or rough matte surfaces, etc., and it is difficult to meet the market demand for unique decorative effects and diverse textures.
[0003] However, some existing glaze firing methods with special effects either cannot precisely control the particle morphology and distribution of the glaze, resulting in unstable product quality and poor appearance effects; or in the process of pursuing unique effects, they ignore the cleaning problem of the glaze during actual use, making the product prone to dirt accumulation, bringing inconvenience to consumers. In addition, in terms of technology, traditional firing methods do not control key factors such as temperature and atmosphere finely enough, and it is difficult to achieve precise shaping of the glaze during the melting process, thus unable to stably produce ceramic products with high-quality bead-like granular frosted glaze surfaces. Moreover, there is a lack of in-depth research and effective utilization of the action mechanisms of the various components in the glaze formula, making it difficult to precisely regulate the physical and chemical properties of the glaze, such as surface tension, etc., during the firing process, thereby affecting the formation and quality of the bead-like particles. Therefore, there is an urgent need for a firing method for a bead-like granular frosted glaze surface that has a uniform bead-like granular frosted glaze surface, and combines good light transmittance and easy-cleaning characteristics.
[0004] Currently, there is an urgent need for a firing method for a bead-like granular frosted glaze surface that has a uniform bead-like granular frosted glaze surface, and combines good light transmittance and easy-cleaning characteristics to meet the urgent market demand for high-quality, beautiful, and practical ceramic products. Therefore, developing a firing method for a bead-like granular frosted glaze surface has important practical significance. To solve the above problems, the present invention proposes a firing method for a bead-like granular frosted glaze surface. Summary of the Invention
[0005] The technical problem to be solved by the present invention is: to provide a firing method for a bead-like granular frosted glaze surface that has a uniform bead-like granular frosted glaze surface, and combines good light transmittance and easy-cleaning characteristics to meet the urgent market demand for high-quality, beautiful, and practical ceramic products.
[0006] To solve the above technical problems, the present invention is solved by the following technical solutions: A firing method for bead-shaped granular frosted glaze, comprising the following steps: Step 1, blank production and pigment painting: The blank is prepared by conventional ceramic forming processes, such as slip casting, dry pressing, or isostatic pressing, etc., into the required shape and size. The formed blank is dried to a certain extent to ensure it has appropriate strength and water absorption. Using ceramic pigments, according to the designed pattern, it is decorated on the surface of the blank by hand painting such as painting, calligraphy, etc. or machine printing such as screen printing, inkjet printing, etc. The pigments should be selected for high temperature resistance and good compatibility with the glaze and the blank to ensure that there will be no problems such as color change, peeling, or chemical reactions during the subsequent firing process. The pattern should be clear and complete, laying the foundation for the decorative effect of the final product; Step 2, preparation of granular glaze layer raw materials: Accurately weigh each raw material: SiO2 accounts for 60% - 70%, Al2O3 accounts for 17% - 19%, K2O accounts for 4% - 6%, Na2O accounts for 1% - 3%, component A accounts for 2% - 3%, and the remaining oxides account for 4% - 7%. Among them, SiO2 is the main glass former, providing the basic framework structure of the glaze layer; Al2O3 helps to improve the hardness and wear resistance of the glaze layer; K2O and Na2O act as fluxes, reducing the melting temperature of the glaze; the remaining oxides may include CaO, MgO, Fe2O3, etc., which can adjust the color, luster, and physical properties of the glaze, etc. Component A is a special composite additive, mainly composed of appropriate amounts of titanium dioxide (TiO2) and boron oxide (B2O3). TiO2 can increase the surface energy of the glaze at high temperatures, prompting the glaze molecules to tend to form droplet-like shapes with larger surface tension, while B2O3 can reduce the viscosity of the glaze, making the glaze flow and spread more easily at high temperatures, and also helps to synergistically act with other components to enhance the surface tension, so that the molten glaze forms smooth granular beads during the firing process; Step 3, preparation of granular glaze slurry: Put the weighed glaze layer raw materials into a ball mill, add alumina balls as the ball milling medium, and use water as the grinding aid for ball milling. The weight ratio of raw material: ball: water is strictly controlled within the range of 1:1 - 2:2 - 4. The ball milling time is determined according to the fineness requirements of the raw materials and the efficiency of the ball mill, generally 6 - 10 hours. The glaze water obtained after ball milling is filtered to remove impurities, and then the water content of the glaze water is adjusted to 60% - 72% by adding water or evaporation concentration to make it have an appropriate consistency for subsequent glazing operations, and at the same time ensure that the glaze slurry can form uniform granular particles when sprayed; Step 4, Granular nozzle adjustment: Select a suitable glazing nozzle and adjust parameters such as the nozzle aperture, pressure, and spraying angle according to the properties of the glaze slurry and the required particle size requirements. Through experiments and optimization, the glaze is ejected from the nozzle in a uniform granular state. When it adheres to the surface of the green body, it can form an obvious granular feeling, and the particle size meets the 200-mesh standard, that is, the minimum outer diameter of the particles is greater than 0.8 mm, and the minimum distance between particles is 1 mm, providing a guarantee for obtaining a uniform and beautiful bead-like granular matte glaze surface; Step 5, Priming glaze application: Prepare ordinary glaze water, and its composition can be selected according to the basic performance requirements of the product, such as using traditional feldspar glaze or lime glaze, etc. Slowly immerse the green body in the ordinary glaze water to ensure that the surface of the green body is fully wetted and a uniform layer of primer glaze is attached. The dipping time is determined according to the water absorption of the green body and the concentration of the glaze water, generally 15 - 45 seconds. After dipping, place the green body in a well-ventilated environment with relatively stable temperature and humidity and let it stand for 10 - 60 minutes to allow the excess glaze to drain naturally, avoiding defects such as uneven glaze layer thickness or running glaze, and ensuring the flatness and uniformity of the primer glaze layer; Step 6, Glazing: Use a professional glazing machine to evenly spray the adjusted granular glaze slurry on the green body that has been applied with the primer glaze. During the spraying process, keep the running speed of the glazing machine stable. According to the shape and size of the green body, reasonably adjust the spraying distance and angle, and spray the green body comprehensively and evenly. For circular green bodies, spray evenly around its circumference; for flat green bodies, spray the entire surface carefully to ensure that the granularity of the sprayed glaze is uniform and the distribution density is consistent, forming a granular glaze surface with a moderate thickness and uniform particle distribution; Step 7, Preliminary firing: Put the glazed green body into an electric kiln and select a reducing or oxidizing atmosphere for firing. When using an oxidizing atmosphere in the electric kiln for firing, the specific steps are as follows: At the beginning of firing, open the kiln door with a gap of 5 - 10 cm to allow the moisture and a small amount of organic matter in the green body and glaze to slowly escape. The temperature starts from room temperature and rises to 300 °C at a rate of 1 - 1.5 °C per minute, and fire for 150 - 180 min. This stage is mainly to remove the free water and part of the crystal water in the green body and glaze, and at the same time, preliminarily sinter the green body to enhance its strength; Then, the temperature rises to 300 - 600 °C at a rate of 1.2 - 1.8 °C per minute and fires for 120 - 150 min. At this time, the organic matter in the green body is further decomposed and oxidized, and some components in the glaze start to undergo solid-phase reactions, such as the decomposition of carbonates and sulfates, etc., to prepare for the subsequent high-temperature melting; Then, the temperature rises to 600 - 750 °C at a rate of 0.8 - 1.2 °C per minute and fires for 50 - 70 min. By gradually increasing the temperature, the moisture in the glaze and green body is gradually removed, and at the same time, some low-melting-point substances in the glaze start to melt, and the glaze layer starts to be preliminarily melted and combined with the green body to form a preliminary glaze surface structure; Step 8. Advanced firing: When the temperature rises to 750°C, close the kiln door to gradually stabilize the atmosphere inside the kiln and enter the high-temperature firing stage. The temperature rises from 750°C to 1100°C at a rate of 2 - 2.5°C per minute and is fired for 80 - 110 minutes. In this stage, most of the components in the glaze start to melt. Due to the action of component A, the surface tension of the molten glaze gradually increases and begins to show a tendency to aggregate and form bead-like dots. The synergistic effect of TiO2 and B2O3 changes the intermolecular interaction force of the glaze, increases the surface energy, thus promoting the glaze to form independent droplet-shaped particles. At the same time, B2O3 also ensures a certain degree of fluidity of the glaze, making the particle distribution more uniform. Then, the temperature rises to 1100 - 1260°C at a rate of 1.5 - 2°C per minute and is fired for 120 - 170 minutes. At this time, the glaze is completely melted and forms smooth bead-like particles under the action of surface tension, which are evenly distributed on the surface of the green body, forming a unique frosted glaze effect. When the temperature reaches 1260°C, keep it warm for 15 - 30 minutes to fully melt and homogenize the glaze, ensure that the shape and distribution of the bead-like particles are more stable and uniform, then stop firing, open the kiln door, leave a 3 - 5 cm gap, and let the kiln cool naturally to gradually solidify the glaze, thereby obtaining a ceramic product with a frosted glaze surface of bead-like particles.
[0007] Preferably, for the preparation of the granular glaze layer raw materials: accurately weigh each raw material: Component Ratio SiO2 60%~70% Al2O3 17%~19% K2O 4%~6% Na2O 1%~3% Component A 2%~3% Other oxides 4%~7% Preferably, component A mainly contains appropriate metal oxides such as titanium dioxide (TiO2) and calcium oxide (CaO). During the high-temperature firing process, TiO2 can reduce the melt viscosity of the glaze and at the same time increase its surface energy, changing the intermolecular interaction force of the glaze molecules and tending to form droplet shapes with a larger surface tension. CaO can chemically react with other components in the glaze to generate some compounds with high melting points and low surface tension coefficients. These compounds play a "pinning" role in the glaze melt, further preventing the excessive spreading of the molten glaze, thereby enhancing the overall surface tension and promoting the glaze to form smooth bead-like particles at high temperatures, ultimately achieving the unique effect of a frosted glaze surface of bead-like particles.
[0008] Preferably, in the preliminary firing step, the heating rate from room temperature to 300°C is 1 - 2°C per minute, the heating rate from 300°C to 600°C is 1.5 - 2°C per minute, and the heating rate from 600°C to 750°C is 1 - 1.5°C per minute. Component A includes TiO2 and CaO, where TiO2 accounts for 60% - 70% of the weight of component A, and CaO accounts for 30% - 40% of the weight of component A.
[0009] Preferably, in the advanced firing step, the heating rate from 750 °C to 1100 °C is 2-3 °C per minute, and the heating rate from 1100 °C to 1260 °C is 1.5-2.5 °C per minute. In the preparation step of the granular glaze slurry, the ball milling time is 8-12 hours.
[0010] Preferably, in the step of adjusting the granular nozzle, the particle size of the fired glaze is 200 mesh, the minimum outer diameter of the glaze particles is 0.5 mm, the height of the bulged granular glaze is about 0.4 mm. The glaze particles are relatively large and have good light transmittance, so that the pigments on the surface of the underlying green body can be seen. There are no large cleaning dead corners on the granular glaze surface, which is suitable for hand washing or machine washing.
[0011] Preferably, the ordinary glaze water is a conventional basic glaze in the ceramic field, and its function is to provide an attachment basis for the granular glaze surface and enhance the overall stability and durability of the glaze surface. In the step of adjusting the granular nozzle, the glaze is ejected in a granular form by adjusting the aperture, pressure and spraying angle of the nozzle. Among them, the nozzle aperture is 1-1.5 mm, the pressure is 0.3-0.5 MPa, and the spraying angle is 40-50 degrees.
[0012] Preferably, in the step of applying the bottom glaze, the immersion time in the bottom glaze water is 20-40 seconds. In the step of spraying glaze, the spraying speed of the spraying machine is 8-12 cm per minute.
[0013] Preferably, in the preliminary firing step, the heating rate from room temperature to 300 °C is 1-2 °C per minute, the heating rate from 300-600 °C is 1.5-2 °C per minute, and the heating rate from 600-750 °C is 1-1.5 °C per minute. In the S51 step, the heating rate from 750-1100 °C is 2-3 °C per minute, and the heating rate from 1100-1260 °C is 1.5-2.5 °C per minute.
[0014] Preferably, the glaze particles on the surface of the ceramic product have good light transmittance, so that the pigments on the surface of the underlying green body can be seen. There are no large cleaning dead corners on the granular glaze surface, which is suitable for hand washing or machine washing. The particle size of the fired glaze is 200 mesh, the minimum outer diameter of the glaze particles is 0.5 mm, and the height of the bulged granular glaze is about 0.4 mm.
[0015] Compared with the prior art, the present invention has the following beneficial effects: 1. The firing method of the bead-shaped granular matte glaze of the present invention. In terms of the glaze quality, by precisely controlling the firing process and raw material formula, the precise control of the glaze particle size has been successfully achieved. After firing, the glaze particle size stably reaches the expected 200 mesh, and the minimum outer diameter of the glaze particles is 0.5 mm. This uniform and fine particle distribution makes the glaze surface present a unique and beautiful texture, giving people a high-quality feeling both visually and tactilely, greatly enhancing the artistic appreciation and decoration of ceramic products, meeting the aesthetic needs of modern consumers for personalized and delicate ceramic products, and providing strong support for the application of ceramic products in the high-end decoration field. It has broad market prospects in art ceramic ornaments, high-grade tableware, and architectural decorative ceramics, etc.; 2. The firing method of the bead-shaped granular matte glaze of the present invention. The glaze surface has excellent light transmittance. Due to the careful regulation of the glaze particle size, larger glaze particles can allow light to penetrate better while ensuring the stability of the glaze surface structure, thus clearly showing the pigment patterns painted on the surface of the underlying body. This not only enriches the artistic expression form of ceramic products, enabling them to present a unique color layering and three-dimensional sense, but also provides more possibilities and creative space for ceramic art creation. Applying the glaze of the present invention to a ceramic vase painted with delicate traditional Chinese fine brushwork can make the picture show a hazy and elegant beauty through the glaze layer, as if giving the painting a unique filter effect, further enhancing the cultural and artistic connotation and collection value of ceramic products, making ceramic products not only practical utensils but also artworks with cultural inheritance significance; 3. The firing method of the bead-shaped granular matte glaze of the present invention. From the perspective of practicality, the design with the bulging height of the granular glaze being about 0.4 mm effectively avoids the problem of difficult-to-clean dead corners caused by too high glaze particles. For ceramic tableware such as plates and bowls for daily use, this characteristic greatly reduces the cleaning difficulty. Whether it is hand-washing or machine-washing, it can be easily handled without leaving dirt due to the glaze structure, ensuring the hygienic cleanliness of the tableware, significantly improving the practicality and ease of use of ceramic products in daily life, making the ceramic products of the present invention have stronger market competitiveness in fields such as families and the catering industry, being able to better meet the needs of consumers for ceramic products that combine beauty and practicality, solving the cleaning problems of traditional granular glaze ceramic products, and providing technical guarantee for the large-scale popularization and use of ceramic tableware, and is expected to promote the development of the entire ceramic tableware industry towards higher quality and easier cleaning; 4. The firing method of the bead-shaped granular frosted glaze of the present invention has good controllability and repeatability. By specifying in detail each step from blank production to firing completion, including the precise proportioning of raw materials, ball milling parameters, glazing methods, as well as the temperature curve, atmosphere control, and kiln door operation during the firing process, etc., the entire production process can be carried out under strict process standards, effectively reducing the product quality fluctuation problems caused by unstable processes, improving production efficiency and product qualification rate, reducing production costs and rejection rates. It is of great significance for large-scale industrial production of ceramic products. It can help enterprises improve production efficiency, enhance market competitiveness, and promote the sustainable development of the ceramic industry while ensuring product quality. At the same time, it also provides a reliable basis and reference for the further research and improvement of related technologies, promotes the continuous development of ceramic firing technology, and expands its application potential in more fields. For example, in the surface treatment of industrial ceramics, electronic ceramics and other fields, the technical idea of the present invention may provide useful reference and inspiration for solving similar glaze preparation problems. Detailed implementation mode
[0016] Unless otherwise clearly specified in the context, nouns without quantifiers and nouns modified by "the" include singular and plural referents.
[0017] As used in the specification and claims of this application, the terms "comprising", "including", "having", "can", "containing" and their variants are open transitional phrases, terms or words that mean the need to have the specified components / steps and allow the existence of other components / steps. However, such descriptions should also be interpreted as describing the composition or method as "consisting of" and "consisting essentially of" the listed components / steps, which allows only the specified components / steps and any inevitable impurities that may result therefrom, and excludes other components / steps.
[0018] The numerical values in the specification and claims of this application should be understood to include the same numerical values when reduced to the same number of significant figures and numerical values that differ from the said values by less than the experimental error of the conventional measurement techniques used to determine the said values of the type described in this application.
[0019] All ranges disclosed herein include the indicated endpoints and can be combined independently (for example, the range of "2 grams to 10 grams" includes the endpoints 2 grams and 10 grams, and all intermediate values).
[0020] The terms "about" and "approximate" may be used to include any numerical value that can vary without changing the basic function of that value. When used with a range, "about" and "approximate" also disclose the range defined by the absolute values of the two endpoints. For example, "about 2 to about 4" also discloses the range "2 to 4". Generally, the terms "about" and "approximate" may refer to ±10% of the indicated number. However, for temperature, the term "about" means ±1°C.
[0021] Unless otherwise expressly specified, percentages of elements shall be considered as weight percentages of the alloy.
[0022] This disclosure may relate to the temperature of certain method steps. It should be noted that these indicators generally refer to the temperature set by a heat source (such as a furnace), rather than necessarily the temperature that the heated material must reach.
[0023] The following description is used to disclose the present invention and enable those skilled in the art to implement the present invention. The preferred embodiments in the following description are only examples, and those skilled in the art can think of other obvious variations. The basic principles of the present invention defined in the following description can be used in other embodiments, variations, improvements, equivalent solutions, and other technical solutions without departing from the spirit and scope of the present invention.
[0024] Example 1 In the steps of blank making and pigment painting, a round ceramic dinner plate blank is formed by manual throwing, and a beautiful floral pattern is painted on the surface of the blank using blue ceramic pigment; Preparation of granular glaze layer raw materials: Accurately weigh SiO2: 65%, Al2O3: 18%, K2O: 5%, Na2O: 2%, Component A (where TiO2: 1.5%, CaO: 0.5%), and the remaining oxides (mainly Fe2O3, MgO, etc., a total of 4.5%), and mix them thoroughly; Preparation of granular glaze slurry: Put the mixed raw materials into a ball mill and ball mill for 10 hours according to the weight ratio of raw materials: balls: water of 1:1.5:3. After ball milling, adjust the water content of the glaze water to 65% to obtain glaze water with a suitable consistency; Adjustment of granular nozzle: Adjust the nozzle aperture to 1.2 mm, set the pressure to 0.4 MPa, and the spraying angle to 45 degrees, so that the glaze is sprayed out in a uniform granular shape, and the granular feeling on the surface of the blank is obvious, and the particle size meets the requirements of 200 mesh; Application of bottom glaze: Immerse the blank in ordinary transparent glaze water for 30 seconds to ensure that a layer of bottom glaze is attached to the surface of the blank by infiltration, and then let it stand for 30 minutes to drain the excess glaze; Spraying glaze: Use a glaze spraying machine to spray the glaze slurry on the blank at a uniform speed of 10 cm per minute to form a granular glaze surface and ensure uniform spraying; Initial firing: Fired in an electric kiln under an oxidizing atmosphere. When initially firing, leave a 8-cm gap for the kiln door. Heat the temperature from room temperature to 300 °C at a rate of 1.5 °C per minute and fire for 160 min; heat the temperature to 300 - 600 °C at a rate of 1.8 °C per minute and fire for 130 min; heat the temperature to 600 - 750 °C at a rate of 1.2 °C per minute and fire for 60 min. Advanced firing: When the temperature rises to 750 °C, close the kiln door. Heat the temperature from 750 °C to 1100 °C at a rate of 2.5 °C per minute and fire for 90 min; heat the temperature to 1100 - 1260 °C at a rate of 2 °C per minute and fire for 150 min; when the temperature is 1260 °C, keep it warm for 20 min and then stop firing. Open the kiln door with a 4-cm gap and let it cool naturally. The glaze bead particles on the finally obtained ceramic dinner plate are plump, evenly distributed, have good light transmittance, the pigment pattern is clearly visible, the particle height is moderate, and it is easy to clean.
[0025] Example 2 For the square ceramic vase blank, in the blank making and pigment painting steps, use the machine printing method to print an abstract geometric pattern on the surface of the blank and use yellow ceramic pigment. Preparation of granular glaze layer raw materials: SiO2: 62%, Al2O3: 17.5%, K2O: 4.5%, Na2O: 1.5%, Component A (where TiO2: 1.2%, CaO: 0.8%), the remaining oxides (mainly ZnO, MnO, etc., a total of 5.5%). Subsequent parameters for the preparation of granular glaze slurry, adjustment of granular nozzles, application of bottom glaze, spraying glaze, and firing steps are finely adjusted according to the blank shape and actual requirements. For example, the nozzle aperture is adjusted to 1 mm, the pressure is set to 0.35 MPa, the bottom dipping glaze time is 40 seconds, let it stand for 40 minutes, and the spraying glaze speed is adjusted to 8 cm per minute, etc. The finally fired ceramic vase has a unique granular matte effect on the glaze surface, complements the geometric pattern, shows an elegant artistic style, and also has good practicality.
[0026] Example 3 Blank making and pigment painting: Select high-quality kaolin and use the traditional manual throwing process to make a circular ceramic dinner plate blank with a diameter of 20 cm. After the blank is formed, use blue ceramic pigment and hand-paint a delicate flower and bird pattern on the surface of the blank to ensure that the pigment adheres evenly and the pattern lines are clear and smooth. Preparation of granular glaze layer raw materials: Accurately weigh the following raw materials: 65% SiO2, 18% Al2O3, 5% K2O, 2% Na2O, Component A (consisting of 1.5% TiO2 and 0.5% ZrO2), and the remaining oxides (including 3% CaO, 2% MgO, and 2% Fe2O3). Thoroughly mix these raw materials in a stirrer for 30 minutes to ensure uniform distribution, and set aside for later use; Preparation of granular glaze slurry: Put the mixed glaze layer raw materials into a ball mill, add alumina balls as the ball milling medium, and use water as the grinding aid. Conduct ball milling according to the weight ratio of raw materials: balls: water of 1:1.5:3, and set the ball milling time to 10 hours to fully refine the raw materials. The glaze water obtained after ball milling is adjusted to a water content of 65% by adding an appropriate amount of water to obtain glaze water with a suitable consistency for subsequent glazing operations; Adjustment of granular nozzle: Select a circular nozzle with a pore diameter of 1.2 mm, install it on the glazing equipment, and adjust the air pressure of the glazing equipment to 0.4 MPa so that the glaze material sprays out of the nozzle in a uniform granular form. Conduct a trial spray on a test blank, observe the adhesion of the glaze material particles, and adjust the distance between the nozzle and the blank to 30 cm to ensure that when the glaze material particles adhere to the surface of the blank, they have an obvious granular feeling and the particle size meets the 200-mesh requirement (the minimum outer diameter of the particles is greater than 0.8 mm, and the minimum distance between the particles is 1 mm); Application of the bottom glaze: Slowly immerse the dinner plate blank with the pattern drawn into ordinary transparent glaze water, and control the glazing time within 20 seconds to ensure that the surface of the blank is evenly wetted and adheres to a layer of bottom glaze material. After glazing, place the blank vertically on a well-ventilated shelf and let it stand for 20 minutes to allow the excess glaze material to drain naturally, avoiding uneven glaze layer thickness; Glazing: Use a glazing machine to evenly spray the adjusted granular glaze slurry on the blank. Set the running speed of the glazing machine to 10 cm per minute so that the glaze slurry can evenly cover the surface of the blank to form a granular glaze surface. For a circular dinner plate blank, spray around its circumference to ensure uniform spraying and consistent particle size; Initial firing: Put the glazed green body into an electric kiln and fire it under an oxidizing atmosphere. At the beginning of the initial firing, open the kiln door with a gap of 8 cm to allow the moisture and a small amount of organic matter in the green body and glaze to slowly escape. The temperature starts from room temperature and rises to 300 °C at a rate of 1.5 °C per minute, and fire for 160 min; then, the temperature rises to 300 - 600 °C at a rate of 1.8 °C per minute and fire for 130 min; then, the temperature rises to 600 - 750 °C at a rate of 1.2 °C per minute and fire for 60 min. During the entire initial firing process, do not add any other gases, and only heat through the heating elements of the electric kiln to gradually discharge the moisture and organic matter in the green body and glaze. At the same time, the glaze starts to undergo preliminary reactions and sintering; Advanced firing: When the temperature rises to 750 °C, close the kiln door to stabilize the atmosphere in the kiln and enter the high-temperature firing stage. The temperature rises from 750 °C to 1100 °C at a rate of 2.5 °C per minute and fire for 90 min; at this stage, most of the components in the glaze start to melt, and due to the action of TiO2 and ZrO2 in component A, the surface tension of the molten glaze gradually increases. TiO2 can reduce the melt viscosity of the glaze and at the same time increase its surface energy, changing the intermolecular interaction force of the glaze molecules and tending to form droplet-like shapes with a larger surface tension; ZrO2 reacts with other components in the glaze at high temperatures to form some compounds with high melting points and low surface tension coefficients, which play a "pinning" role in the glaze melt and further prevent the excessive spreading of the molten glaze, thus enhancing the overall surface tension. Then, the temperature rises to 1100 - 1260 °C at a rate of 2 °C per minute and fire for 150 min. At this time, the glaze is completely melted and forms smooth bead-shaped particles under the action of surface tension, evenly distributed on the surface of the green body, forming a unique frosted glaze effect. When the temperature reaches 1260 °C, hold for 20 min to allow the glaze to fully melt and homogenize, ensuring that the shape and distribution of the bead particles are more stable and uniform. Then stop firing, open the kiln door with a 4 cm gap, and let the kiln cool naturally to allow the glaze to gradually solidify, thereby obtaining a ceramic dinner plate with a frosted glaze surface with bead particles;
[0027] After testing, the particle size of the glaze of the fired dinner plate is 200 mesh, and the minimum outer diameter of the glaze particles is 0.5 mm. Due to controlling the particle size of the glaze, the particles of the glaze are relatively large and have good light transmittance, and the flower and bird patterns drawn on the surface of the underlying green body can be clearly seen. The height of the bulging of the granular glaze is about 0.4 mm, without excessive protrusions, so that there are no large cleaning dead corners in the granular glaze surface. For the cleaning of the dinner plate, whether it is hand-washing or machine-washing, the impact is relatively small.
[0028] Example 4 Green body production and pigment painting: A square ceramic decorative ornament blank with a side length of 15 cm is made by a mechanical forming process. Using green ceramic pigments, a modern geometric pattern is printed on the surface of the blank by machine printing. The pattern coverage rate is about 50%, ensuring that the pigment is tightly combined with the blank, with no obvious color difference and defects. Preparation of the raw materials for the granular glaze layer: Weigh 62% of SiO2, 17.5% of Al2O3, 4.5% of K2O, 1.5% of Na2O, component A (composed of 1.2% of TiO2 and 0.8% of CeO2), and the remaining oxides (including 2.5% of CaO, 2% of ZnO, and 1.5% of MnO). Put these raw materials into a high-speed mixer and stir for 40 minutes to make them fully and evenly mixed. Preparation of the granular glaze slurry: Put the mixed raw materials into a ball mill and ball mill for 12 hours according to the weight ratio of raw materials: balls: water of 1:1.2:2.5. After ball milling, adjust the moisture content of the glaze water to 68% by evaporation concentration to obtain glaze water with a suitable consistency. Adjustment of the granular nozzle: Select a nozzle with a pore diameter of 1 mm, install it on the intelligent glazing equipment, and by adjusting the equipment parameters, set the glazing air pressure to 0.35 MPa and the distance between the nozzle and the blank to 25 cm, so that the glaze material is ejected in a uniform granular shape. Observe the particle adhesion on the test blank to ensure that the particle size meets the 200-mesh requirement (the minimum outer diameter of the particles is greater than 0.8 mm, and the minimum distance between the particles is 1 mm), and the adhesion effect is good, with an obvious sense of granularity. Application of the bottom glaze: Immerse the blank in ordinary white glaze water for 30 seconds to ensure that a layer of bottom glaze material adheres to the surface of the blank by infiltration. After immersion glazing, place the blank in a dry and ventilated environment and let it stand for 30 minutes to drain the excess glaze material, ensuring that the thickness of the bottom glaze material is uniform. Glazing: Use a glazing machine to perform glazing operations on the blank. Set the running speed of the glazing machine to 8 cm per minute and spray the blank evenly on the whole surface to ensure that the glaze material particle size is evenly distributed on the surface of the blank, forming a complete granular glaze surface. Initial firing: Put the glazed green body into an electric kiln and fire it in an oxidizing atmosphere. When initially firing, leave a 6-cm gap for the kiln door to be open. Raise the temperature from room temperature to 300 °C at a rate of 1.2 °C per minute and fire for 170 minutes; then, raise the temperature to 300 - 600 °C at a rate of 1.6 °C per minute and fire for 140 minutes; then, raise the temperature to 600 - 750 °C at a rate of 1 °C per minute and fire for 65 minutes. During the entire initial firing process, no additional gas is added, and heating is only carried out by relying on the heating system of the electric kiln itself to gradually expel the moisture and organic matter in the green body and glaze, enabling the glaze to undergo preliminary reaction and sintering; Advanced firing: When the temperature rises to 750 °C, close the kiln door. Raise the temperature from 750 °C to 1100 °C at a rate of 2.2 °C per minute and fire for 100 minutes; at this stage, due to the action of TiO₂ and CeO₂ in component A, the surface tension of the glaze gradually increases. TiO₂ reduces the melt viscosity and increases the surface energy, promoting the glaze to form a droplet shape; CeO₂ reacts with other components at high temperature, changing the physical and chemical properties of the glaze and enhancing the surface tension. Then, raise the temperature to 1100 - 1260 °C at a rate of 1.8 °C per minute and fire for 160 minutes. At this time, the glaze is completely melted and forms bead-shaped particles, evenly distributed on the surface of the green body. When the temperature reaches 1260 °C, keep it warm for 25 minutes to fully melt and homogenize the glaze, then stop firing, open the kiln door with a 3-cm gap, and let it cool naturally to obtain a ceramic decorative ornament with a unique bead-shaped granular frosted glaze surface.
[0029] After testing, the particle size of the glaze of the fired decorative ornament is 200 mesh, the minimum outer diameter of the glaze particles is 0.5 mm, the glaze particles are relatively large, with good light transmittance, and the geometric patterns below are clearly visible, increasing the artistic beauty of the decorative ornament. The height of the bulging of the granular glaze is about 0.4 mm, which is convenient to clean. Whether it is daily wiping or simple cleaning, it will not cause cleaning difficulties due to the glaze surface particles, meeting the market demand for high-quality and easy-to-clean ceramic decorative ornaments.
[0030] Example 5. A firing method for a bead-shaped granular frosted glaze surface, comprising the following steps: Step 1. Blank production and pigment drawing: The green body is prepared by conventional ceramic forming processes, such as slip casting, dry pressing, or isostatic pressing, etc., into the required shape and size. After forming, the green body is dried to a certain extent to ensure that it has appropriate strength and water absorption; Use ceramic pigments and decorate the surface of the green body by hand painting (such as painting, calligraphy, etc.) or machine printing (such as screen printing, inkjet printing, etc.) according to the designed pattern. Pigments should be selected with high temperature resistance and good compatibility with glazes and green bodies to ensure that no problems such as color change, peeling, or chemical reactions occur during subsequent firing. The pattern should be clear and complete, laying the foundation for the decorative effect of the final product; Step 2: Preparation of granular glaze layer raw materials: Accurately weigh each raw material: SiO2 accounts for 60% - 70%, Al2O3 accounts for 17% - 19%, K2O accounts for 4% - 6%, Na2O accounts for 1% - 3%, Component A accounts for 2% - 3%, and the remaining oxides account for 4% - 7%. Among them, SiO2 is the main glass former, providing the basic framework structure of the glaze layer; Al2O3 helps to improve the hardness and wear resistance of the glaze layer; K2O and Na2O act as fluxes, reducing the melting temperature of the glaze; the remaining oxides may include CaO, MgO, Fe2O3, etc., which can adjust the color, luster, and physical properties of the glaze, etc.; Component A is a special composite additive, mainly composed of appropriate amounts of titanium dioxide (TiO2) and boron oxide (B2O3). TiO2 can increase the surface energy of the glaze at high temperatures, prompting the glaze molecules to tend to form droplet shapes with larger surface tension, while B2O3 can reduce the viscosity of the glaze, making the glaze flow and spread more easily at high temperatures. At the same time, it also helps to synergistically act with other components to enhance the surface tension, so that the molten glaze forms smooth granular beads during the firing process; Step 3: Preparation of granular glaze slurry: Put the weighed glaze layer raw materials into a ball mill, add alumina balls as the ball milling medium, and use water as the grinding aid for ball milling. The weight ratio of raw materials: balls: water is strictly controlled within the range of 1:1 - 2:2 - 4. The ball milling time is determined according to the fineness requirements of the raw materials and the efficiency of the ball mill, generally 6 - 10 hours; The glaze water obtained after ball milling is filtered to remove impurities, and then the water content of the glaze water is adjusted to 60% - 72% by adding water or evaporation concentration to make it have an appropriate consistency, facilitating subsequent glazing operations, and at the same time ensuring that the glaze slurry can form uniform particles when sprayed out; Step 4: Adjustment of granular nozzle: Select a suitable glaze spraying nozzle, and adjust parameters such as the nozzle aperture, pressure, and spraying angle according to the properties of the glaze slurry and the required particle size requirements. Through experiments and optimization, the glaze is sprayed out of the nozzle in the form of uniform particles. When attached to the surface of the green body, it can form an obvious particle feeling, and the particle size meets the 200 - mesh standard (that is, the minimum outer diameter of the particles is greater than 0.8mm, and the minimum distance between particles is 1mm), providing a guarantee for obtaining a uniform and beautiful bead - like granular matte glaze surface; Step Five: Glazing the bottom layer: Prepare ordinary glaze water, and its composition can be selected according to the basic performance requirements of the product. For example, traditional feldspar glaze or lime glaze can be used. Slowly immerse the green body into the ordinary glaze water to ensure that the surface of the green body is fully wetted and a uniform bottom layer of glaze is attached. The dipping time is determined according to the water absorption of the green body and the concentration of the glaze water, generally 15 - 45 seconds; After dipping, place the green body in a well-ventilated environment with relatively stable temperature and humidity and let it stand for 10 - 60 minutes to allow the excess glaze to drain naturally, avoiding defects such as uneven glaze layer thickness or running glaze, and ensuring the flatness and uniformity of the bottom layer of glaze; Step Six: Spraying glaze: Use a professional glaze spraying machine to evenly spray the adjusted granular glaze slurry on the green body that has been glazed with the bottom layer of glaze. During the spraying process, keep the running speed of the glaze spraying machine stable. According to the shape and size of the green body, reasonably adjust the spraying distance and angle to spray the green body comprehensively and evenly. For circular green bodies, spray evenly around its circumference; for flat green bodies, spray the entire surface carefully to ensure that the granularity of the sprayed glaze is uniform and the distribution density is consistent, forming a granular glaze surface with a moderate thickness and uniform particle distribution; Step Seven: Preliminary firing: Put the glazed green body into an electric kiln and select a reducing or oxidizing atmosphere for firing. In this embodiment, the electric kiln is fired in an oxidizing atmosphere. The specific steps are as follows: During the initial firing, open the kiln door and leave a gap of 5 - 10 cm so that the moisture and a small amount of organic matter in the green body and glaze can be slowly discharged. The temperature starts from room temperature and rises to 300°C at a rate of 1 - 1.5°C per minute, and fire for 150 - 180 minutes. This stage is mainly to remove the free water and part of the crystal water in the green body and glaze, and at the same time preliminarily sinter the green body to enhance its strength; Then, the temperature rises to 300 - 600°C at a rate of 1.2 - 1.8°C per minute and fires for 120 - 150 minutes. At this time, the organic matter in the green body is further decomposed and oxidized, and some components in the glaze start to undergo solid-phase reactions, such as the decomposition of carbonates and sulfates, etc., to prepare for the subsequent high-temperature melting; Then, the temperature rises to 600 - 750°C at a rate of 0.8 - 1.2°C per minute and fires for 50 - 70 minutes. By gradually raising the temperature, the moisture in the glaze and green body is gradually discharged, and at the same time, some low-melting-point substances in the glaze start to melt, and the glaze layer starts to be preliminarily melted and combined with the green body to form a preliminary glaze surface structure; Step Eight: Advanced firing: When the temperature rises to 750°C, close the kiln door to make the atmosphere in the kiln gradually stable and enter the high-temperature firing stage; The temperature is raised from 750 °C to 1100 °C at a rate of 2 - 2.5 °C per minute and fired for 80 - 110 min. In this stage, most of the components in the glaze start to melt, and due to the action of component A, the surface tension of the molten glaze gradually increases, and a tendency to aggregate and form bead-like dots begins to appear. The synergistic effect of TiO2 and B2O3 changes the intermolecular interaction force of the glaze, increasing the surface energy, thus promoting the formation of independent droplet-shaped particles in the glaze. At the same time, B2O3 also ensures a certain degree of fluidity of the glaze, making the particle distribution more uniform; Then, the temperature is raised to 1100 - 1260 °C at a rate of 1.5 - 2 °C per minute and fired for 120 - 170 min. At this time, the glaze is completely melted and forms smooth bead-shaped particles under the action of surface tension, which are evenly distributed on the surface of the green body, forming a unique frosted glaze effect; When the temperature reaches 1260 °C, it is held for 15 - 30 min to fully melt and homogenize the glaze, ensuring that the shape and distribution of the bead-shaped particles are more stable and uniform. Then the fire is stopped, the kiln door is opened, leaving a 3 - 5 cm gap, and the kiln is allowed to cool naturally, enabling the glaze to gradually solidify, thereby obtaining a ceramic product with a frosted glaze surface of bead-shaped particles.
[0031] The specific steps are as follows: First, the green body is prepared by conventional ceramic forming processes, such as slip casting, dry pressing, or isostatic pressing, etc., to form the required shape and size. The formed green body is dried to a certain extent to ensure it has appropriate strength and water absorption. Ceramic pigments are used, and according to the designed pattern, they are decorated on the surface of the green body by hand painting, such as painting, calligraphy, etc., or machine printing, such as screen printing, inkjet printing, etc. The pigments should be selected with high temperature resistance and good compatibility with the glaze and the green body to ensure that there will be no problems such as color change, peeling, or chemical reactions during the subsequent firing process. The pattern should be clear and complete, laying the foundation for the decorative effect of the final product. At this time, the staff accurately weighs each raw material: SiO2 accounts for 60% - 70%, Al2O3 accounts for 17% - 19%, K2O accounts for 4% - 6%, Na2O accounts for 1% - 3%, component A accounts for 2% - 3%, and the remaining oxides account for 4% - 7%. Among them, SiO2 is the main glass former, providing the basic framework structure of the glaze layer; Al2O3 helps to improve the hardness and wear resistance of the glaze layer; K2O and Na2O act as fluxes, reducing the melting temperature of the glaze; the remaining oxides may include CaO, MgO, Fe2O3, etc., which can adjust the color, luster, and physical properties of the glaze. Component A is a special composite additive, mainly composed of appropriate amounts of titanium dioxide (TiO2) and boron oxide (B2O3). TiO2 can increase the surface energy of the glaze at high temperatures, prompting the glaze molecules to tend to form droplet-like shapes with larger surface tension, while B2O3 can reduce the viscosity of the glaze, making the glaze flow and spread more easily at high temperatures, and also helps to cooperate with other components to enhance the surface tension, so that the molten glaze forms smooth granular bead-like shapes during the firing process. At this time, the staff puts the weighed glaze raw materials into a ball mill, adds alumina balls as the ball milling medium, and uses water as the grinding aid for ball milling. The weight ratio of raw material: ball: water is strictly controlled within the range of 1:1 - 2:2 - 4. The ball milling time is determined according to the fineness requirements of the raw materials and the efficiency of the ball mill, generally 6 - 10 hours. The glaze water obtained after ball milling is filtered to remove impurities, and then the water content of the glaze water is adjusted to 60% - 72% by adding water or evaporation concentration to make it have an appropriate consistency for subsequent glazing operations, and at the same time ensure that the glaze slurry can form uniform particles when sprayed out. At this time, the staff selects a suitable glazing nozzle and adjusts parameters such as the aperture, pressure, and spraying angle of the nozzle according to the properties of the glaze slurry and the required particle size requirements. Through experiments and optimizations, the glaze is sprayed out of the nozzle in the form of uniform particles, and when attached to the surface of the green body, it can form an obvious particle feeling, and the particle size meets the 200-mesh standard, that is, the minimum outer diameter of the particles is greater than 0.8 mm, and the minimum distance between the particles is 1 mm, which provides a guarantee for obtaining a uniform and beautiful bead-like granular matte glaze surface. At this time, the staff prepares ordinary glaze water, and its composition can be selected according to the basic performance requirements of the product. For example, traditional feldspar glaze or lime glaze can be used. Slowly immerse the green body into the ordinary glaze water to ensure that the surface of the green body is fully wetted and a uniform bottom glaze layer is attached. The dipping time is determined according to the water absorption of the green body and the concentration of the glaze water, generally 15 - 45 seconds. After dipping, place the green body in a well-ventilated environment with relatively stable temperature and humidity and let it stand for 10 - 60 minutes to allow the excess glaze to drain naturally, avoiding defects such as uneven glaze layer thickness or running glaze, and ensuring the flatness and uniformity of the bottom glaze layer; At this time, the staff uses a professional spraying machine to evenly spray the adjusted granular glaze slurry on the green body that has been applied with the bottom glaze. During the spraying process, keep the running speed of the spraying machine stable. According to the shape and size of the green body, reasonably adjust the spraying distance and angle to spray the green body comprehensively and evenly. For circular green bodies, spray evenly around its circumference; for flat green bodies, spray the entire surface carefully to ensure that the sprayed glaze particles are uniform in size and consistent in distribution density, forming a granular glaze surface with a moderate thickness and uniform particle distribution; At this time, the staff puts the glazed green body into an electric kiln and selects a reducing or oxidizing atmosphere for firing. When firing in an oxidizing atmosphere in the electric kiln, the specific steps are as follows: At the initial firing, open the kiln door with a gap of 5 - 10 cm to allow the moisture and a small amount of organic matter in the green body and glaze to slowly escape. The temperature starts from room temperature and rises to 300 °C at a rate of 1 - 1.5 °C per minute and is fired for 150 - 180 min. This stage is mainly to remove the free water and part of the crystal water in the green body and glaze, and at the same time preliminarily sinter the green body to enhance its strength; Then, the temperature rises to 300 - 600 °C at a rate of 1.2 - 1.8 °C per minute and is fired for 120 - 150 min. At this time, the organic matter in the green body further decomposes and oxidizes, and some components in the glaze start to undergo solid-phase reactions, such as the decomposition of carbonates and sulfates, to prepare for the subsequent high-temperature melting; Then, the temperature rises to 600 - 750 °C at a rate of 0.8 - 1.2 °C per minute and is fired for 50 - 70 min. By gradually raising the temperature, the moisture in the glaze and green body is gradually removed, and at the same time, some low-melting-point substances in the glaze start to melt, and the glaze layer starts to preliminarily melt and combine with the green body to form a preliminary glaze surface structure. Finally, when the temperature rises to 750 °C, the staff closes the kiln door to make the atmosphere in the kiln gradually stable and enter the high-temperature firing stage. The temperature rises from 750 °C at a rate of 2 - 2.It is heated to 1100 °C at a rate of 5 °C, and fired for 80 - 110 min. At this stage, most of the components in the glaze start to melt. Due to the action of component A, the surface tension of the molten glaze gradually increases, and a tendency to aggregate and form bead-like dots begins to appear. The synergistic effect of TiO2 and B2O3 changes the intermolecular interaction force of the glaze, increasing the surface energy, thus promoting the formation of independent droplet-shaped particles of the glaze. At the same time, B2O3 also ensures a certain degree of fluidity of the glaze, making the particle distribution more uniform; then, the temperature is raised to 1100 - 1260 °C at a rate of 1.5 - 2 °C per minute, and fired for 120 - 170 min. At this time, the glaze is completely melted and formed under the action of surface tension.
[0032] Those skilled in the art should understand that the embodiments of the present invention shown in the above description are only examples and do not limit the present invention. The object of the present invention has been fully and effectively achieved. The functions and structural principles of the present invention have been shown and described in the embodiments. Without departing from the said principles, the embodiments of the present invention can have any deformation or modification. Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents. This specific embodiment is only an interpretation of the present application and does not limit the present application. Those skilled in the art can make modifications without creative contributions to this embodiment according to needs after reading this specification, but as long as it is within the scope of the claims of the present application, it is protected by the patent law.
Claims
1. A method for firing a beaded granular frosted glaze, characterized in that: The following steps are involved: Step 1, blank preparation and pigment painting: the blank is prepared by conventional ceramic molding process, such as slip injection molding, dry pressing molding or isostatic pressing molding, etc., into the required shape and size. The formed blank is dried to a certain degree to ensure that it has appropriate strength and water absorption. Ceramic pigments are used to decorate the surface of the blank according to the design pattern by hand painting such as painting, calligraphy, etc. or machine printing such as screen printing, inkjet printing, etc. The pigment should be selected to be high temperature resistant and compatible with the glaze and blank to ensure that there will be no discoloration, shedding or chemical reaction during the subsequent firing process. The pattern should be clear and complete, laying the foundation for the decorative effect of the final product; Step 2, preparation of raw materials for granular glaze layer: accurately weigh the raw materials: SiO2 accounts for 60% to 70%, Al2O3 accounts for 17% to 19%, K2O accounts for 4% to 6%, Na2O accounts for 1% to 3%, component A accounts for 2% to 3%, and the remaining oxides account for 4% to 7%. Among them, SiO2 is the main glass former, providing the basic skeleton structure of the glaze layer; Al2O3 helps to improve the hardness and wear resistance of the glaze layer; K2O and Na2O act as flux to reduce the melting temperature of the glaze; the remaining oxides may include CaO, MgO, Fe2O3, etc. , they can adjust the color, gloss and physical properties of the glaze. Component A is a special composite additive, mainly composed of appropriate amounts of titanium dioxide (TiO2) and boron oxide (B2O3). TiO2 can increase the surface energy of the glaze at high temperatures, causing the glaze molecules to tend to form droplets with large surface tension, while B2O3 can reduce the viscosity of the glaze, making it easier to flow and spread at high temperatures. It also helps to work synergistically with other ingredients to enhance surface tension, so that the molten glaze forms smooth beads during the firing process. Step 3, preparation of granular glaze slurry: weigh the glaze layer raw materials and put them into a ball mill, add alumina balls as ball milling media, and use water as a grinding aid for ball milling. The weight ratio of raw materials: balls: water is strictly controlled within the range of 1:1-2:2-4. The ball milling time is determined according to the fineness requirements of the raw materials and the efficiency of the ball mill, generally 6-10 hours. The glaze water obtained after ball milling is filtered to remove impurities, and then the water content of the glaze water is adjusted to 60% to 72% by adding water or evaporation concentration to make it have an appropriate consistency, which is convenient for subsequent glazing operations and ensures that the glaze slurry can form uniform particles when sprayed out; Step 4, particle nozzle adjustment: select a suitable glaze spraying nozzle, and adjust the parameters such as nozzle aperture, pressure and spray angle according to the properties of the glaze slurry and the required particle size requirements. Through experiments and optimization, the glaze is sprayed from the nozzle in a uniform particle shape. When attached to the surface of the blank, it can form a clear particle feeling, and the particle size meets the 200 mesh standard, that is, the minimum outer diameter of the particles is greater than 0.8mm, and the minimum spacing between the particles is 1mm, which provides a guarantee for obtaining a uniform and beautiful beaded particle frosted glaze surface; Step 5, bottom glazing: prepare ordinary glaze water, the composition of which can be selected according to the basic performance requirements of the product, such as traditional feldspar glaze or lime glaze, slowly immerse the body into the ordinary glaze water to ensure that the surface of the body is fully infiltrated and adhered with a uniform layer of bottom glaze. The glazing time is determined according to the water absorption of the body and the concentration of the glaze water, generally 15 to 45 seconds. After glazing, place the body in a well-ventilated environment with relatively stable temperature and humidity for 10 to 60 minutes to allow the excess glaze to drain naturally, avoid defects such as uneven glaze thickness or glaze flow, and ensure the flatness and uniformity of the bottom glaze; Step 6, glaze spraying: Use a professional glaze spraying machine to evenly spray the adjusted granular glaze slurry on the body that has been applied with the bottom glaze. During the spraying process, keep the running speed of the glaze spraying machine stable. According to the shape and size of the body, reasonably adjust the spraying distance and angle, and spray the body comprehensively and evenly. For a round body, spray it at a uniform speed around it; for a flat body, spray the entire surface carefully to ensure that the glaze spraying particle size is uniform and the distribution density is consistent, forming a layer of granular glaze with moderate thickness and uniform particle distribution; Step 7, preliminary firing: put the glazed body into the electric kiln and select reducing or oxidizing atmosphere for firing. The specific steps are as follows: during the initial firing, the kiln door is opened, leaving a gap of 5-10cm so that the moisture and a small amount of organic matter in the body and glaze can be slowly discharged. The temperature starts from room temperature and rises to 300℃ at a rate of 1-1.5℃ per minute. The firing is 150-180min. This stage is mainly to remove the free water and part of the crystal water in the body and glaze, and at the same time make the body initially sintered to enhance its strength; then, the temperature is raised at a rate of 1.2-1.8℃ per minute. ℃ to 300-600℃, and fired for 120-150min. At this time, the organic matter in the body is further decomposed and oxidized, and some components in the glaze begin to undergo solid-phase reactions, such as the decomposition of carbonates and sulfates, to prepare for subsequent high-temperature melting; then, the temperature is raised to 600-750℃ at a rate of 0.8-1.2℃ per minute, and fired for 50-70min. By gradually raising the temperature, the moisture in the glaze and the body is gradually discharged. At the same time, some low-melting-point substances in the glaze begin to melt, and the glaze layer begins to melt initially and combine with the body to form a preliminary glaze surface structure; Step 8: Advanced firing: When the temperature rises to 750℃, close the kiln door to stabilize the atmosphere in the kiln and enter the high-temperature firing stage. The temperature rises from 750℃ to 1100℃ at a rate of 2-2.5℃ per minute and is fired for 80-110min. At this stage, most of the components in the glaze begin to melt, and due to the effect of component A, the surface tension of the molten glaze gradually increases, and it begins to show a tendency to aggregate and form beads. The synergistic effect of TiO2 and B2O3 changes the interaction force between glaze molecules and increases the surface energy, thereby prompting the glaze to form independent droplet-shaped particles. At the same time, B2O3 also ensures that the glaze is to a certain extent The fluidity is improved to make the particle distribution more uniform; then, the temperature is raised to 1100-1260℃ at a rate of 1.5-2℃ per minute and fired for 120-170min. At this time, the glaze is completely melted and forms smooth bead-shaped particles under the action of surface tension, which are evenly distributed on the surface of the body to form a unique frosted glaze effect; when the temperature reaches 1260℃, keep warm for 15-30min to make the glaze fully melted and homogenized, ensuring that the shape and distribution of the bead-shaped particles are more stable and uniform, then stop firing, open the kiln door, leave a gap of 3-5cm, let the kiln cool down naturally, and make the glaze gradually solidify, so as to obtain ceramic products with bead-shaped granular frosted glaze.
2. The method for firing a beaded granular frosted glaze surface according to claim 1, characterized in that: Preparation of the raw materials for the granular glaze layer: Accurately weigh the raw materials:
3. The method for firing a beaded granular frosted glaze according to claim 1, characterized in that: The component A mainly comprises appropriate amounts of metal oxides such as titanium dioxide (TiO2) and calcium oxide (CaO). During the high-temperature firing process, TiO2 can reduce the melt viscosity of the glaze and increase its surface energy, thereby changing the interaction force between the glaze molecules and tending to form droplets with larger surface tension. CaO can react chemically with other components in the glaze to generate some compounds with high melting points and low surface tension coefficients. These compounds play a "pinning" role in the glaze melt, further preventing the excessive spreading of the molten glaze, thereby enhancing the overall surface tension and prompting the glaze to form smooth bead-shaped particles at high temperature, ultimately achieving the unique effect of bead-shaped granular frosted glaze.
4. The method for firing a beaded granular frosted glaze surface according to claim 1, characterized in that: In the preliminary firing step, the heating rate from room temperature to 300°C is 1-2°C per minute, the heating rate from 300°C to 600°C is 1.5-2°C per minute, and the heating rate from 600°C to 750°C is 1-1.5°C per minute. The component A includes TiO2 and CaO, wherein TiO2 accounts for 60% to 70% of the weight of component A, and CaO accounts for 30% to 40% of the weight of component A.
5. The method for firing a beaded granular frosted glaze surface according to claim 1, characterized in that: In the advanced firing step, the heating rate from 750°C to 1100°C is 2-3°C per minute, and the heating rate from 1100°C to 1260°C is 1.5-2.5°C per minute. In the preparation step of the granular glaze slurry, the ball milling time is 8-12 hours.
6. The method for firing a beaded granular frosted glaze surface according to claim 1, characterized in that: In the particle nozzle adjustment step, the particle size of the fired glaze is 200 mesh, the minimum outer diameter of the glaze particles is 0.5 mm, the height of the bulging particle glaze is about 0.4 mm, the particles of the glaze are large and have good light transmittance, and the pigment on the surface of the blank below can be seen. The particle glaze surface does not have a large cleaning dead angle and is suitable for hand washing or machine washing.
7. The method for firing a beaded granular frosted glaze surface according to claim 1, characterized in that: The ordinary glaze is a conventional basic glaze in the ceramic field, and its function is to provide an adhesion basis for the granular glaze surface and enhance the overall stability and durability of the glaze surface. In the particle nozzle adjustment step, the glaze is sprayed in a granular state by adjusting the nozzle aperture, pressure and spray angle, wherein the nozzle aperture is 1-1.5mm, the pressure is 0.3-0.5MPa, and the spray angle is 40-50 degrees.
8. The method for firing a beaded granular frosted glaze surface according to claim 1, characterized in that: In the bottom glazing step, the time for immersing the bottom layer in glaze water is 20 to 40 seconds, and in the glazing step, the spraying speed of the glaze sprayer is 8 to 12 cm per minute.
9. The method for firing a beaded granular frosted glaze surface according to claim 1, characterized in that: In the preliminary firing step, the heating rate from room temperature to 300°C is 1-2°C per minute, the heating rate from 300-600°C is 1.5-2°C per minute, and the heating rate from 600-750°C is 1-1.5°C per minute. In the S51 step, the heating rate from 750-1100°C is 2-3°C per minute, and the heating rate from 1100-1260°C is 1.5-2.5°C per minute.
10. The method for firing a beaded granular frosted glaze surface according to claim 1, characterized in that: The glaze particles on the surface of the ceramic product have good light transmittance, so the pigment on the surface of the green body below can be seen, and the granular glaze surface does not have a large cleaning dead angle, and is suitable for hand washing or machine washing. The glaze particle size after firing is 200 mesh, the minimum outer diameter of the glaze particles is 0.5mm, and the height of the bulging granular glaze is about 0.4mm.