Heat-resistant impact-resistant environment-friendly ceramic and preparation method thereof

By modifying tantalum carbide whiskers and synergistically combining components, the problems of thermal shock resistance and dispersion bonding in daily-use ceramics have been solved, achieving a balance between high performance and environmental protection, and improving the durability and safety of ceramics.

CN121085613BActive Publication Date: 2026-02-17FUJIAN DEHUA GENTLE CERAMICS
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Patent Information

Application Number
CN202511643495.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-11-11
Publication Date
2026-02-17
Estimated Expiration
2045-11-11

AI Technical Summary

Technical Problem

Traditional daily-use ceramics are brittle and have poor thermal shock resistance. Furthermore, the problems of high-performance whisker dispersion and interfacial bonding in ceramic blanks have not been effectively solved, making it difficult to meet the market demands for durability and environmental health.

Method used

Modified tantalum carbide whiskers are used, and the whisker dispersion problem is solved by hydroxylation, silane coupling and surface-initiated free radical polymerization modification. A strong interfacial bond is built in situ during high-temperature sintering. Combined with components such as nano-titanium dioxide and hollow glass microspheres, low-temperature sintering and photocatalytic self-cleaning are achieved.

Benefits of technology

It significantly improves the heat resistance, shock resistance, and environmental protection properties of ceramics, reduces sintering energy consumption, ensures effective bonding between the reinforcement and the matrix, enhances toughness and thermal shock resistance, and also possesses photocatalytic self-cleaning function.

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Abstract

The application discloses a kind of heat-resistant impact-resistant environment-friendly ceramic and preparation method thereof, it is related to domestic ceramic technical field, the environment-friendly ceramic is made of the following components by weight fraction: kaolin 20~50 parts, potassium feldspar 5~20 parts, sodium feldspar 5~20 parts, 3~12 parts of medical stone, spinel 2~8 parts, nano titanium dioxide 15~30 parts, modified carbide tantalum whisker 6~12 parts, hollow glass microsphere 4~10 parts, lithium chloride 2~5 parts, silane coupling agent 1~3 parts;The application introduces a kind of specially modified carbide tantalum whisker, solves the problem of whisker dispersion when low-temperature mixing, and in-situ constructs firm interface bonding when high-temperature sintering, so that the toughening potential of whisker is fully stimulated, and the ceramic is endowed with excellent heat-resistant impact-resistant performance;At the same time, the whole formula is synergistic, has the energy-saving of low-temperature sintering and the environmental protection characteristics of photocatalytic self-cleaning, realizes the unity of high performance and green environmental protection.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of ceramics, in particular to a heat-resistant and impact-resistant environment-friendly ceramic and a preparation method thereof. BACKGROUND

[0002] Daily-use ceramic products, as essential utensils in people's daily life, are applied to tableware, tea sets, cooking utensils, etc. With the improvement of living quality, consumers' requirements for daily-use ceramics have long been beyond simple holding and decoration functions, and higher expectations for durability, safety and convenience of use have been put forward.

[0003] However, traditional daily-use ceramics generally have an inherent defect, i.e., high brittleness and poor thermal shock resistance. In daily use, ceramic tableware often produces notches or even breaks due to inadvertent bumps and collisions during stacking, greatly shortening its service life. More seriously, in the kitchen environment, ceramic utensils need to frequently withstand severe temperature changes, such as directly washing a porcelain bowl containing hot soup with cold water, or directly placing a cold storage utensil taken from the refrigerator into a microwave oven for heating. Such "thermal shock" can easily cause the ceramic to crack or burst, not only causing economic losses, but also possibly causing safety hazards such as scalding.

[0004] In order to improve the strength and toughness of daily-use ceramics, the prior art usually adopts methods such as optimizing the body formula and adjusting the firing system, but these improvements are relatively limited in improving the impact resistance and thermal shock resistance of the material, and it is difficult to fundamentally solve the problem. Although whisker reinforcement is a mature toughening method in the field of special industrial ceramics, its application in the field of daily-use ceramics faces many challenges. First, high-performance whiskers such as tantalum carbide (TaC) have strong chemical inertness and poor compatibility with traditional ceramic body materials, making it difficult to form effective interface bonding. Second, whiskers are prone to agglomeration in ceramic slurry, and if not evenly dispersed, they will become internal defects of the product, affecting product quality.

[0005] In addition, modern home concepts also pay more and more attention to health and environmental protection. Traditional ceramics have high firing temperatures and high energy consumption; at the same time, the cleanliness of the surface of tableware is directly related to the health of the user. Therefore, developing a new type of durable and environment-friendly ceramic that can resist daily bumps and cold-heat shocks, and has low-temperature energy-saving firing and self-cleaning and other environmentally friendly and healthy characteristics, has become an important development direction for the upgrading and replacement of the daily-use ceramics industry to meet new market demands.

[0006] In summary, how to effectively apply the reinforcement theory of high-performance whiskers to the production practice of daily-use ceramics, overcome the dispersion and interface bonding problems of whiskers, and significantly improve the durability and thermal shock resistance of household ceramics while ensuring safety and environmental protection, is a technical problem to be solved in the field. SUMMARY

[0007] In order to solve the problems in the prior art, the present application provides a heat-resistant and impact-resistant environment-friendly ceramic and a preparation method thereof, which introduces a specially modified tantalum carbide whisker to solve the problem of whisker dispersion during low-temperature mixing and construct a firm interface during high-temperature sintering, thereby fully stimulating the toughening potential of the whisker and endowing the ceramic with excellent heat-resistant and impact-resistant properties; meanwhile, the overall formula is synergistic, has the energy-saving property of low-temperature sintering and the environment-friendly property of photocatalytic self-cleaning, and realizes the unification of high performance and green environmental protection.

[0008] In order to achieve the above object, the present application adopts the following technical scheme:

[0009] A heat-resistant and impact-resistant environment-friendly ceramic is prepared from the following components in parts by weight: 20-50 parts of kaolin, 5-20 parts of potassium feldspar, 5-20 parts of sodium feldspar, 3-12 parts of medical stone, 2-8 parts of spinel, 15-30 parts of nano titanium dioxide, 6-12 parts of modified tantalum carbide whisker, 4-10 parts of hollow glass microbeads, 2-5 parts of lithium chloride and 1-3 parts of silane coupling agent.

[0010] Preferably, the modified tantalum carbide whisker is prepared by the following method steps:

[0011] (1) dispersing the tantalum carbide whisker into hydrogen peroxide, ultrasonic treatment, stirring reaction, centrifuging, washing and drying the product to obtain activated tantalum carbide whisker;

[0012] Hydroxylation of tantalum carbide whisker: the mechanism of this step is to introduce high-activity hydroxyl (-OH) on the surface of inert tantalum carbide (TaC) whisker by using the strong oxidizing property of hydrogen peroxide. Under the assistance of heating and ultrasonic energy, the hydrogen peroxide is decomposed or directly reacts with the Ta atoms or naturally existing oxide layer (Ta-O-Ta) on the surface of the whisker to form a dense, chemically bonded hydroxyl functional group (Ta-OH) on the surface of the whisker. These newly generated hydroxyl groups "activate" the originally inert surface and make it become a reaction site capable of subsequent chemical grafting.

[0013] Preferably, in step (1), the purity of the tantalum carbide whisker is ≥98%, the diameter is 0.3-0.6 μm, and the aspect ratio is >10.

[0014] Preferably, in step (1), the amount ratio of tantalum carbide to hydrogen peroxide is 10 g: 100-200 mL, and the concentration of hydrogen peroxide is 20-30 wt%.

[0015] Preferably, in step (1), the ultrasonic treatment is performed for 10-30 min, and the stirring reaction conditions are stirring at 60-90 °C for 2-5 h.

[0016] (2) dispersing the activated tantalum carbide whisker into anhydrous ethanol, ultrasonic treatment, then adding KH570 and a small amount of deionized water, reflux reaction, centrifuging, washing and drying the product to obtain the pretreated tantalum carbide whisker;

[0017] Silane coupling: this step uses KH-570 as a "molecular bridge" for covalent grafting. First, the methoxysilane end of the KH-570 molecule undergoes a hydrolysis reaction catalyzed by a small amount of deionized water, and is converted into an extremely unstable silanol end . Subsequently, this newly generated silanol group will undergo a dehydration condensation reaction with the hydroxyl groups (Ta-OH) on the surface of the activated whisker to form a very stable and firm "Ta-O-Si" covalent bond, successfully introducing polymerizable reactive sites to the surface of the whisker.

[0018] Preferably, in step (2), the amount ratio of the activated tantalum carbide whisker, anhydrous ethanol, KH570 and deionized water is 10g: 100-200mL: 0.5-2g: 1-5mL.

[0019] Preferably, in step (2), the ultrasonic treatment is 10-30min; the reflux reaction conditions are refluxing at 65-80℃ for 6-12h.

[0020] (3) dispersing the pretreated tantalum carbide whisker into DMF, ultrasonic treatment, then adding acryloyloxyethyl trimethyl ammonium chloride, acrylic cage polysilsesquioxane, adding AIBN under a nitrogen atmosphere, stirring reaction, centrifuging, washing and drying the product to obtain the modified tantalum carbide whisker.

[0021] Surface-initiated radical polymerization: the initiator AIBN is degraded under heating to generate primary radicals in the solution. These radicals will attack and open the carbon-carbon double bond carried by KH-570 anchored on the surface of the whisker, thereby transferring and fixing the radical active center to the surface of the whisker. Subsequently, this surface active center will continuously capture and add acryloyloxyethyl trimethyl ammonium chloride and acrylic cage polysilsesquioxane monomers from the solution, allowing the polymer chains to "grow" from the surface of the whisker, thereby obtaining the final core-shell structure modified tantalum carbide whisker.

[0022] Preferably, in step (3), the amount ratio of the pretreated tantalum carbide whisker, DMF, acryloyloxyethyl trimethyl ammonium chloride, acrylic cage polysilsesquioxane and AIBN is 10g: 100-200mL: 4-10g: 2-5g: 0.1-0.4g.

[0023] Preferably, in step (3), the ultrasonic treatment is 10-30min; the stirring reaction conditions are stirring at 70-85℃ for 6-24h.

[0024] Preferably, the silane coupling agent is at least one of an amino silane coupling agent, an epoxy silane coupling agent.

[0025] The application also claims a method for preparing the heat-resistant and impact-resistant environment-friendly ceramic, comprising the following steps: mixing 20-50 parts of kaolin, 5-20 parts of potassium feldspar, 5-20 parts of sodium feldspar, 3-12 parts of medical stone and 2-8 parts of spinel to obtain a first mixture; mixing 5-15 parts of nano-titanium dioxide, 6-12 parts of modified tantalum carbide whisker, 4-10 parts of hollow glass microsphere and 2-5 parts of lithium chloride to obtain a second mixture; putting the first mixture, the second mixture and 1-3 parts of silane coupling agent into a ball mill, adding a proper amount of deionized water, grinding for 18-36 hours, removing impurities, pressing mud and refining mud to obtain a blank; pressing the blank into a shape, drying, baking at 850-1000 DEG C for 6-12 hours, cooling to room temperature, glazing the baked product, putting it into a kiln and firing at 1000-1100 DEG C to obtain the heat-resistant and impact-resistant environment-friendly ceramic.

[0026] Compared with the prior art, the application has the following beneficial effects:

[0027] 1. The application provides a heat-resistant and impact-resistant environment-friendly ceramic, and the formula uses kaolin, potassium feldspar and sodium feldspar as the ceramic matrix, which is stable in structure; meanwhile, the strong fluxing agent lithium chloride is introduced, which significantly reduces the sintering temperature of the ceramic and saves the production energy consumption. Secondly, by compounding spinel, modified tantalum carbide whisker and hollow glass microsphere, excellent heat-resistant and impact-resistant performance is achieved: the spinel itself has excellent high-temperature stability and builds a heat-resistant skeleton; the tantalum carbide whisker as a reinforcing phase consumes a large amount of energy through crack deflection and fiber bridging mechanisms, effectively inhibits the further expansion of cracks, thereby greatly enhances the toughness of the ceramic and reduces the failure risk under thermal shock and thermal shock; the introduction of the hollow glass microsphere not only reduces the density of the ceramic, but more importantly, the hollow structure provides a thermal stress buffer layer, further improving the thermal shock resistance of the material. In addition, the addition of nano-titanium dioxide endows the ceramic with the environmental protection function of photocatalytic self-cleaning, and the medical stone as a natural mineral filler optimizes the sintering performance and ensures the biological safety of the product. Finally, the silane coupling agent realizes the effective interface combination of each inorganic component and the modified whisker, ensures the efficient transmission of stress and maximizes the advantages of each component.

[0028] 2、The application provides a preparation method of modified tantalum carbide whiskers, a first step of hydroxylation and a second step of silane coupling, successfully converting the originally inert and easy-to-agglomerate tantalum carbide whisker surface into an active platform with polymerization reaction anchor points, preliminarily improving the dispersibility of the whisker in a solvent. A third step in-situ grows a copolymer "soft shell" composed of two functional monomers on the whisker surface. The introduced acryloyloxyethyl trimethyl ammonium chloride (AETAC) segment brings positive charges to the whisker surface, greatly inhibits the agglomeration and sedimentation of the whisker in the ceramic slurry through electrostatic repulsion, and significantly improves the forming fluidity of the slurry and the density of the final body; and the grafted polyhedral oligomeric silsesquioxane (POSS) plays a key role in secondary reinforcement, which will be in-situ converted into nanoceramic structure in subsequent high-temperature sintering, and tightly adheres to the surface of the tantalum carbide whisker to form a high-temperature-resistant and oxidation-resistant "ceramic interfacial layer". The organic polymer layer will be orderly decomposed and ablated during the ceramic sintering process, and converted into a permanent, chemically bonded, excellent inorganic interfacial layer, perfectly solving the bonding problem of the reinforcing body and the matrix, ensuring efficient stress transmission, so as to fully stimulate the reinforcing and toughening potential of the whisker. DETAILED DESCRIPTION

[0029] In order to make the purpose, technical scheme and advantages of the present application clearer, the present application will be further described in detail below with examples. Of course, the specific examples described herein are only used to explain the present application, and are not used to limit the present application.

[0030] Unless otherwise specified, the chemical reagents and materials in the present application are purchased through market channels or synthesized from raw materials purchased through market channels.

[0031] Acryloyloxyethyl trimethyl ammonium chloride (AETAC), CAS: 1620202-27-8;

[0032] Hollow glass microspheres are purchased from 3M Company, USA, model K46.

[0033] A preparation method of a heat-resistant and impact-resistant environment-friendly ceramic comprises the following steps:

[0034] (1) 10 g of tantalum carbide whiskers are dispersed into 100-200 mL of 20-30 wt% hydrogen peroxide, ultrasonic treatment is performed for 10-30 min, and stirring reaction is performed at 60-90 DEG C for 2-5 h, then the product is centrifuged, washed and dried to obtain activated tantalum carbide whiskers;

[0035] (2) 10 g of the activated tantalum carbide whisker is dispersed into 100-200 mL of anhydrous ethanol, ultrasonic treatment is conducted for 10-30 min, then 0.5-2 g of KH570 and 1-5 mL of deionized water are added, reflux reaction is conducted at 65-80 °C for 6-12 h, the product is centrifuged, washed and dried to obtain the pretreated tantalum carbide whisker;

[0036] (3) 10 g of the pretreated tantalum carbide whisker is dispersed into 100-200 mL of DMF, ultrasonic treatment is conducted for 10-30 min, then 4-10 g of acryloyloxyethyl trimethyl ammonium chloride and 2-5 g of acryl-caged polysilsesquioxane are added, 0.1-0.4 g of AIBN is added under a nitrogen atmosphere, stirring reaction is conducted at 70-85 °C for 6-24 h, the product is centrifuged, washed and dried to obtain the modified tantalum carbide whisker;

[0037] (4) 20-50 parts of kaolin, 5-20 parts of potassium feldspar, 5-20 parts of sodium feldspar, 3-12 parts of maifanite and 2-8 parts of spinel are mixed to obtain a first mixture; 5-15 parts of nano titanium dioxide, 6-12 parts of the modified tantalum carbide whisker, 4-10 parts of hollow glass microspheres and 2-5 parts of lithium chloride are mixed to obtain a second mixture; the first mixture, the second mixture and 1-3 parts of a silane coupling agent are put into a ball mill, a proper amount of deionized water is added, grinding is conducted for 18-36 h, impurities are removed, the mud is pressed and refined to obtain a blank; the blank is pressed into a shape, dried, subjected to a preliminary firing at 850-1000 °C for 6-12 h, cooled to room temperature, glazed, and sent into a kiln to be fired at 1000-1100 °C to obtain the heat-resistant and impact-resistant environment-friendly ceramic.

[0038] The application will be further described below through specific examples. Example 1

[0039] A preparation method of a heat-resistant and impact-resistant environment-friendly ceramic comprises the following steps:

[0040] (1) 10 g of tantalum carbide whisker is dispersed into 150 mL of 25 wt% hydrogen peroxide, ultrasonic treatment is conducted for 20 min, stirring reaction is conducted at 90 °C for 2 h, the product is centrifuged, washed and dried to obtain the activated tantalum carbide whisker;

[0041] (2) 10 g of the activated tantalum carbide whisker is dispersed into 150 mL of anhydrous ethanol, ultrasonic treatment is conducted for 20 min, then 2 g of KH570 and 5 mL of deionized water are added, reflux reaction is conducted at 80 °C for 6 h, the product is centrifuged, washed and dried to obtain the pretreated tantalum carbide whisker;

[0042] (3) 10 g of the pretreated tantalum carbide whisker was dispersed in 150 mL of DMF, and ultrasonic treatment was performed for 20 min, then 10 g of acryloxyethyl trimethyl ammonium chloride, 5 g of acrylic cage polysilsesquioxane were added, 0.4 g of AIBN was added under a nitrogen atmosphere, and stirring reaction was performed at 85°C for 6 h, the product was centrifuged, washed, and dried to obtain the modified tantalum carbide whisker;

[0043] (4) 5000 g of kaolin, 2000 g of potassium feldspar, 2000 g of sodium feldspar, 1200 g of medical stone, and 800 g of spinel were mixed to obtain a first mixture; 1500 g of nano titanium dioxide, 1200 g of modified tantalum carbide whisker, 1000 g of hollow glass microsphere, and 500 g of lithium chloride were mixed to obtain a second mixture; the first mixture, the second mixture, and 300 g of silane coupling agent KH560 were put into a ball mill, and a proper amount of deionized water was added, and grinding was performed for 24 h, and impurities were removed, and the mud was pressed and refined to obtain a blank; the blank was pressed into a shape, dried, and subjected to a preliminary firing at 950°C for 9 h, and then cooled to room temperature, and glaze was applied to the preliminary fired product, and then the product was put into a kiln and fired at 1050°C to obtain the heat-resistant and impact-resistant environment-friendly ceramic. Example 2

[0044] A method for preparing a heat-resistant and impact-resistant environment-friendly ceramic comprises the following steps:

[0045] (1) 10 g of tantalum carbide whisker was dispersed in 150 mL of 25wt% hydrogen peroxide, and ultrasonic treatment was performed for 20 min, and stirring reaction was performed at 80°C for 3 h, and then the product was centrifuged, washed, and dried to obtain activated tantalum carbide whisker;

[0046] (2) 10 g of the activated tantalum carbide whisker was dispersed in 150 mL of anhydrous ethanol, and ultrasonic treatment was performed for 20 min, then 1.5 g of KH570 and 4 mL of deionized water were added, and reflux reaction was performed at 75°C for 8 h, and then the product was centrifuged, washed, and dried to obtain pretreated tantalum carbide whisker;

[0047] (3) 10 g of the pretreated tantalum carbide whisker was dispersed in 150 mL of DMF, and ultrasonic treatment was performed for 20 min, then 8 g of acryloxyethyl trimethyl ammonium chloride, 4 g of acrylic cage polysilsesquioxane were added, 0.3 g of AIBN was added under a nitrogen atmosphere, and stirring reaction was performed at 80°C for 12 h, and then the product was centrifuged, washed, and dried to obtain modified tantalum carbide whisker;

[0048] (4) 4000 g of kaolin, 1500 g of potassium feldspar, 1500 g of sodium feldspar, 900 g of medical stone, and 600 g of spinel were mixed to obtain a first mixture; 1200 g of nano-titanium dioxide, 1000 g of modified carbonized tantalum whiskers, 800 g of hollow glass beads, and 400 g of lithium chloride were mixed to obtain a second mixture; the first mixture, the second mixture, and 250 g of silane coupling agent KH560 were put into a ball mill, and an appropriate amount of deionized water was added, and grinded for 24 h, impurity removal, mud pressing, and mud refining were performed to obtain a blank; the blank was pressed into a shape, dried, and subjected to a preliminary firing at 950 ℃ for 9 h, cooled to room temperature, glazed on the preliminary fired product, and sent into a kiln to be fired at 1050 ℃, to obtain the heat-resistant and impact-resistant environment-friendly ceramic. Example 3

[0049] A preparation method of a heat-resistant and impact-resistant environment-friendly ceramic, comprising the following steps:

[0050] (1) 10 g of carbonized tantalum whiskers were dispersed into 150 mL of 25 wt% hydrogen peroxide, ultrasonically treated for 20 min, and stirred and reacted at 70 ℃ for 4 h, and the product was centrifuged, washed, and dried to obtain activated carbonized tantalum whiskers;

[0051] (2) 10 g of the activated carbonized tantalum whiskers were dispersed into 150 mL of anhydrous ethanol, ultrasonically treated for 20 min, then 1 g of KH570 and 2 mL of deionized water were added, and the mixture was refluxed and reacted at 70 ℃ for 10 h, and the product was centrifuged, washed, and dried to obtain pretreated carbonized tantalum whiskers;

[0052] (3) 10 g of the pretreated carbonized tantalum whiskers were dispersed into 150 mL of DMF, ultrasonically treated for 20 min, then 6 g of acryloyloxyethyl trimethylammonium chloride and 3 g of acryl-caged polysilsesquioxane were added, 0.2 g of AIBN was added under a nitrogen atmosphere, and the mixture was stirred and reacted at 75 ℃ for 18 h, and the product was centrifuged, washed, and dried to obtain modified carbonized tantalum whiskers;

[0053] (4) 3000 g of kaolin, 1000 g of potassium feldspar, 1000 g of sodium feldspar, 600 g of medical stone, and 400 g of spinel were mixed to obtain a first mixture; 800 g of nano-titanium dioxide, 800 g of modified carbonized tantalum whiskers, 600 g of hollow glass beads, and 300 g of lithium chloride were mixed to obtain a second mixture; the first mixture, the second mixture, and 150 g of silane coupling agent KH560 were put into a ball mill, and an appropriate amount of deionized water was added, and grinded for 24 h, impurity removal, mud pressing, and mud refining were performed to obtain a blank; the blank was pressed into a shape, dried, and subjected to a preliminary firing at 950 ℃ for 9 h, cooled to room temperature, glazed on the preliminary fired product, and sent into a kiln to be fired at 1050 ℃, to obtain the heat-resistant and impact-resistant environment-friendly ceramic. Example 4

[0054] A preparation method of a heat-resistant and impact-resistant environment-friendly ceramic comprises the following steps:

[0055] (1) 10 g of tantalum carbide whiskers are dispersed into 150 mL of 25 wt% hydrogen peroxide, ultrasonic treatment is performed for 20 min, stirring reaction is performed at 60°C for 2 h, the product is centrifuged, washed and dried to obtain activated tantalum carbide whiskers;

[0056] (2) 10 g of the activated tantalum carbide whiskers are dispersed into 150 mL of anhydrous ethanol, ultrasonic treatment is performed for 20 min, then 0.5 g of KH570 and 1 mL of deionized water are added, reflux reaction is performed at 65°C for 12 h, the product is centrifuged, washed and dried to obtain pretreated tantalum carbide whiskers;

[0057] (3) 10 g of the pretreated tantalum carbide whiskers are dispersed into 150 mL of DMF, ultrasonic treatment is performed for 20 min, then 4 g of acryloyloxyethyl trimethyl ammonium chloride and 2 g of acryl-caged polysilsesquioxane are added, 0.1 g of AIBN is added under a nitrogen atmosphere, stirring reaction is performed at 70°C for 24 h, the product is centrifuged, washed and dried to obtain modified tantalum carbide whiskers;

[0058] (4) 2000 g of kaolin, 500 g of potassium feldspar, 500 g of sodium feldspar, 300 g of medical stone and 200 g of spinel are mixed to obtain a first mixture; 500 g of nano-titanium dioxide, 600 g of the modified tantalum carbide whiskers and 400 g of hollow glass microspheres and 200 g of lithium chloride are mixed to obtain a second mixture; the first mixture, the second mixture and 100 g of silane coupling agent KH560 are put into a ball mill, a proper amount of deionized water is added, grinding is performed for 24 h, impurities are removed, the mud is pressed and refined to obtain a blank; the blank is pressed into a shape, dried, subjected to a preliminary firing at 950°C for 9 h, cooled to room temperature, glazed, and sent into a kiln to be fired at 1050°C to obtain the heat-resistant and impact-resistant environment-friendly ceramic. Comparative Example 1

[0059] A preparation method of a heat-resistant and impact-resistant environment-friendly ceramic comprises the following steps:

[0060] (1) 10 g of tantalum carbide whiskers are dispersed into 150 mL of 25 wt% hydrogen peroxide, ultrasonic treatment is performed for 20 min, stirring reaction is performed at 60°C for 2 h, the product is centrifuged, washed and dried to obtain activated tantalum carbide whiskers;

[0061] (2) 10 g of the activated tantalum carbide whiskers are dispersed into 150 mL of anhydrous ethanol, ultrasonic treatment is performed for 20 min, then 0.5 g of KH570 and 1 mL of deionized water are added, reflux reaction is performed at 65°C for 12 h, the product is centrifuged, washed and dried to obtain pretreated tantalum carbide whiskers;

[0062] (3) 10 g of the pretreated tantalum carbide whisker was dispersed into 150 mL of DMF, ultrasonic treatment was performed for 20 min, then 15 g of acryloxyethyl trimethyl ammonium chloride was added, 0.4 g of AIBN was added under a nitrogen atmosphere, and reaction was performed under stirring at 85°C for 6 h. The product was centrifuged, washed, and dried to obtain the modified tantalum carbide whisker;

[0063] (4) 5000 g of kaolin, 2000 g of potassium feldspar, 2000 g of sodium feldspar, 1200 g of medical stone, and 800 g of spinel were mixed to obtain a first mixture; 1500 g of nano-titanium dioxide, 1000 g of the modified tantalum carbide whisker, 200 g of acrylic cage polysilsesquioxane, 1000 g of hollow glass microbeads, and 500 g of lithium chloride were mixed to obtain a second mixture; the first mixture, the second mixture, and 300 g of silane coupling agent KH560 were put into a ball mill, and a proper amount of deionized water was added. Grinding was performed for 24 h, impurities were removed, mud was pressed, and mud was refined to obtain a blank. The blank was pressed into a shape, dried, and subjected to a preliminary firing at 950°C for 9 h. The product was cooled to room temperature, glazed, and sent into a kiln. The product was fired at 1050°C to obtain the heat-resistant and impact-resistant environment-friendly ceramic. Comparative Example 2

[0064] A method for preparing a heat-resistant and impact-resistant environment-friendly ceramic comprises the following steps:

[0065] (1) 10 g of tantalum carbide whisker was dispersed into 150 mL of 25wt% hydrogen peroxide, ultrasonic treatment was performed for 20 min, and reaction was performed under stirring at 90°C for 2 h. The product was centrifuged, washed, and dried to obtain activated tantalum carbide whisker;

[0066] (2) 10 g of the activated tantalum carbide whisker was dispersed into 150 mL of anhydrous ethanol, ultrasonic treatment was performed for 20 min, then 2 g of KH570 and 5 mL of deionized water were added, and reaction was performed under reflux at 80°C for 6 h. The product was centrifuged, washed, and dried to obtain pretreated tantalum carbide whisker;

[0067] (3) 10 g of the pretreated tantalum carbide whisker was dispersed into 150 mL of DMF, ultrasonic treatment was performed for 20 min, then 15 g of acrylic cage polysilsesquioxane was added, 0.4 g of AIBN was added under a nitrogen atmosphere, and reaction was performed under stirring at 85°C for 6 h. The product was centrifuged, washed, and dried to obtain the modified tantalum carbide whisker;

[0068] (4) 5000 g of kaolin, 2000 g of potassium feldspar, 2000 g of sodium feldspar, 1200 g of medical stone, and 800 g of spinel are mixed to obtain a first mixture; 1500 g of nano-titanium dioxide, 1000 g of modified carbonized tantalum whisker, 200 g of acryloyloxyethyl trimethyl ammonium chloride, 1000 g of hollow glass microbeads, and 500 g of lithium chloride are mixed to obtain a second mixture; the first mixture, the second mixture, and 300 g of silane coupling agent KH560 are put into a ball mill, and an appropriate amount of deionized water is added, and grinded for 24 h, impurity removal, mud pressing, and mud refining are performed to obtain a blank; the blank is pressed into a shape, dried, and subjected to a preliminary firing at 950 ℃ for 9 h, cooled to room temperature, glazed, and sent into a kiln to be fired at 1050 ℃ to obtain the heat-resistant and impact-resistant environment-friendly ceramic. Comparative Example 3

[0069] A preparation method of a heat-resistant and impact-resistant environment-friendly ceramic, comprising the following steps:

[0070] (1) 10 g of carbonized tantalum whisker is dispersed into 150 mL of 25 wt% hydrogen peroxide, ultrasonic treatment is performed for 20 min, and stirring reaction is performed at 90 ℃ for 2 h, and the product is centrifuged, washed, and dried to obtain activated carbonized tantalum whisker;

[0071] (2) 10 g of the activated carbonized tantalum whisker is dispersed into 150 mL of anhydrous ethanol, ultrasonic treatment is performed for 20 min, then 2 g of KH570 and 5 mL of deionized water are added, and reflux reaction is performed at 80 ℃ for 6 h, and the product is centrifuged, washed, and dried to obtain pretreated carbonized tantalum whisker;

[0072] (3) 5000 g of kaolin, 2000 g of potassium feldspar, 2000 g of sodium feldspar, 1200 g of medical stone, and 800 g of spinel are mixed to obtain a first mixture; 1500 g of nano-titanium dioxide, 1200 g of pretreated carbonized tantalum whisker, 1000 g of hollow glass microbeads, and 500 g of lithium chloride are mixed to obtain a second mixture; the first mixture, the second mixture, and 300 g of silane coupling agent KH560 are put into a ball mill, and an appropriate amount of deionized water is added, and grinded for 24 h, impurity removal, mud pressing, and mud refining are performed to obtain a blank; the blank is pressed into a shape, dried, and subjected to a preliminary firing at 950 ℃ for 9 h, cooled to room temperature, glazed, and sent into a kiln to be fired at 1050 ℃ to obtain the heat-resistant and impact-resistant environment-friendly ceramic.

[0073] The ceramics prepared in Examples 1-4 and Comparative Examples 1-3 were tested for performance, the apparent porosity was tested according to GB / T 2997-2015 "Test methods of bulk density, apparent porosity and true porosity of dense shaped refractory products", the water absorption was detected according to GB / T 3299-2011 "Method of testing water absorption of ceramic ware", the thermal expansion coefficient was determined according to QB / T 1321-2012 "Method of testing average linear thermal expansion coefficient of ceramic materials", the test temperature range was room temperature-600℃, the lead and cadmium elution (98℃ heating for 1d) was detected according to GB 4806.4-2016 "National food safety standard-Ceramics", the bending strength was tested by using a PT-1036PC universal material testing machine, the sample size was 3mmx4mmx20mm, the span was 16mm, the loading speed of the pressure head was 0.5mm / min, the bending strength was the average value of three measurement results, the fracture toughness was tested according to GB / T 23806-2009 "Method of testing fracture toughness of fine ceramics-SEPB (single edge precracked beam) method", the oxidation resistance was tested by placing the ceramics in 60℃ air for 15d, observing the surface of the ceramics and testing the oxidation resistance, the thermal shock resistance was tested according to GB / T 3298-2022 "Method of testing thermal shock resistance of ceramic ware", the sample was heated to 800℃, then quickly transferred to 25℃ cold water for cooling, the number of times when visible cracks appeared on the sample was recorded, the thermal impact resistance was tested by heating the sample to 800℃, keeping for 30min, then quenching in air, repeating until macroscopic cracks appeared on the sample, the number of times was recorded, and the thermal impact resistance was tested. The specific data are shown in Table 1.

[0074] Table 1: Performance test results of ceramics

[0075]

[0076] The above merely provides the preferred embodiments of the present application, but the protection scope of the present application is not limited thereto, any person skilled in the art can make equivalent substitutions or changes to the technical solutions and the inventive concept of the present application within the technical range disclosed by the present application, which should be covered within the protection scope of the present application.

Claims

1. A heat-resistant, impact-resistant, environmentally friendly ceramic, characterized in that, The components are prepared by weight parts: kaolin 20-50 parts, potassium feldspar 5-20 parts, sodium feldspar 5-20 parts, medical stone 3-12 parts, spinel 2-8 parts, nano titanium dioxide 15-30 parts, modified carbonized tantalum whisker 6-12 parts, hollow glass microsphere 4-10 parts, lithium chloride 2-5 parts, silane coupling agent 1-3 parts; The modified carbonized tantalum whisker is prepared by the following method steps: (1) The carbonized tantalum whisker is dispersed into hydrogen peroxide, ultrasonic treatment, stirring reaction, centrifugation, washing and drying to obtain activated carbonized tantalum whisker; (2) The activated carbonized tantalum whisker is dispersed into anhydrous ethanol, ultrasonic treatment, then KH570 and a small amount of deionized water are added, reflux reaction, centrifugation, washing and drying to obtain pretreated carbonized tantalum whisker; (3) The pretreated carbonized tantalum whisker is dispersed into DMF, ultrasonic treatment, then acryloyloxyethyl trimethyl ammonium chloride, acrylic cage polysilsesquioxane is added, AIBN is added under nitrogen atmosphere, stirring reaction, centrifugation, washing and drying to obtain modified carbonized tantalum whisker.

2. The heat-resistant, impact-resistant, environmentally friendly ceramic according to claim 1, wherein, In step (1), the amount ratio of carbonized tantalum to hydrogen peroxide is 10g:100-200mL; the concentration of hydrogen peroxide is 20-30wt%.

3. The heat-resistant, impact-resistant, environmentally friendly ceramic of claim 1, wherein, In step (1), the ultrasonic treatment is 10-30min; the stirring reaction condition is stirring reaction at 60-90℃ for 2-5h.

4. The heat-resistant, impact-resistant, environmentally friendly ceramic of claim 1, wherein, In step (2), the amount ratio of activated carbonized tantalum whisker, anhydrous ethanol, KH570 and deionized water is 10g:100-200mL:0.5-2g:1-5mL.

5. The heat-resistant, impact-resistant, environmentally friendly ceramic of claim 1, wherein, In step (2), the ultrasonic treatment is 10-30min; the reflux reaction condition is reflux reaction at 65-80℃ for 6-12h.

6. The heat resistant, impact resistant, environmentally friendly ceramic of claim 1, wherein, In step (3), the amount ratio of pretreated carbonized tantalum whisker, DMF, acryloyloxyethyl trimethyl ammonium chloride, acrylic cage polysilsesquioxane and AIBN is 10g:100-200mL:4-10g:2-5g:0.1-0.4g.

7. The heat resistant impact resistant eco-friendly ceramic according to claim 1, wherein, In step (3), the ultrasonic treatment is 10-30min; the stirring reaction condition is stirring reaction at 70-85℃ for 6-24h.

8. The heat resistant, impact resistant, environmentally friendly ceramic of claim 1, wherein, The silane coupling agent is at least one of amino silane coupling agent and epoxy silane coupling agent.

9. A method of preparing a heat-resistant, impact-resistant, environmentally friendly ceramic, characterized by, The method comprises the following steps: mixing kaolin 20-50 parts, potassium feldspar 5-20 parts, sodium feldspar 5-20 parts, medical stone 3-12 parts, spinel 2-8 parts to obtain a first mixture; mixing nano titanium dioxide 5-15 parts, modified carbonized tantalum whisker 6-12 parts, hollow glass microsphere 4-10 parts, lithium chloride 2-5 parts to obtain a second mixture; putting the first mixture, the second mixture and the silane coupling agent 1-3 parts into a ball mill, adding appropriate amount of deionized water, grinding for 18-36h, removing impurities, pressing mud, and practicing mud to obtain a blank; the blank is pressed into shape, dried, fired at 850-1000℃ for 6-12h, cooled to room temperature, glazed on the fired product, sent into a kiln, fired at 1000-1100℃ to obtain the heat-resistant and impact-resistant environment-friendly ceramic; The modified carbonized tantalum whisker is prepared by the following method steps: (1) dispersing the tantalum carbide whisker into hydrogen peroxide, ultrasonic treatment, stirring reaction, centrifuging, washing and drying the product to obtain the activated tantalum carbide whisker; (2) dispersing the activated tantalum carbide whisker into anhydrous ethanol, ultrasonic treatment, then adding KH570 and a small amount of deionized water, refluxing reaction, centrifuging, washing and drying the product to obtain the pretreated tantalum carbide whisker; (3) dispersing the pretreated tantalum carbide whisker into DMF, ultrasonic treatment, then adding acryloyloxyethyl trimethyl ammonium chloride, acrylic cage polysilsesquioxane, adding AIBN under nitrogen atmosphere, stirring reaction, centrifuging, washing and drying the product to obtain the modified tantalum carbide whisker.

Citation Information

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