High-strength ceramic and forming process thereof

Abstract

The invention discloses high-strength ceramic and a forming process thereof, and belongs to the technical field of ceramic materials. The ceramic comprises the following components in parts by mass: 3-10 parts of a reinforcing material, 40-45 parts of kaolin, 25-40 parts of quartz sand, 8-15 parts of aluminum oxide, 3-7 parts of a nano toughening agent and 1-3 parts of pigment. The reinforcing material is # imgabs0, and the heat resistance and the interface bonding force are remarkably improved through the isotope effect of a deuterated group and aryl steric hindrance. The forming process comprises the steps of gradient mixing, ultrasonic-assisted dispersion, high-pressure homogenization and staged curing and sintering, and quenching treatment is introduced to improve the surface density. Meanwhile, the raw material dispersity and the energy consumption efficiency are optimized, the problems that traditional ceramic is low in strength and complex in process are solved, and the high-strength ceramic is applied to special materials for biomedical additive manufacturing.

Description

Technical Field

[0001] The invention relates to the technical field of ceramics, and in particular to a high-strength ceramic and a molding process thereof. Background Art

[0002] In the field of ceramic material technology, traditional ceramic materials have many deficiencies in strength, toughness and processing performance, which limits their widespread use in high-end applications. In the prior art, the strength and toughness of ceramic materials are usually low, which makes it difficult to meet the use requirements in complex mechanical environments, such as artificial joints, dental restorations and orthopedic implants and other biomedical applications. In addition, the preparation process of traditional ceramic materials is complex, energy-intensive and costly, making it difficult to achieve efficient production and large-scale application.

[0003] The lack of strength and toughness of traditional ceramic materials is one of their main technical bottlenecks. Due to the brittle nature of ceramic materials, they are prone to fracture or failure when subjected to high stress or complex mechanical loads. In the prior art, although the toughness of ceramics can be improved to a certain extent by adding toughening agents or optimizing the sintering process, these methods often cannot take into account the comprehensive improvement of strength and toughness at the same time.

[0004] The preparation process of traditional ceramic materials is complex and energy-intensive. In the prior art, the preparation of ceramic materials usually requires high-temperature sintering and multiple treatments, which leads to long production cycles, high energy consumption, and easy introduction of defects such as microcracks and pores, further reducing the mechanical properties of the materials. In addition, traditional processes make it difficult to achieve complex structural design and precise molding of ceramic materials, limiting their application in emerging technologies such as additive manufacturing.

[0005] In summary, ceramic materials in the existing technology have significant deficiencies in strength, toughness, process complexity, energy consumption and cost, and an innovative solution that can comprehensively improve performance, simplify processes and reduce energy consumption is urgently needed. Summary of the invention

[0006] The present invention aims to provide a high-strength ceramic and its forming process to solve the problems of insufficient strength, complex process, high energy consumption and high cost in the prior art. By optimizing the composition and improving the preparation process, the present invention can significantly improve the strength and toughness of the ceramic while reducing production costs and energy consumption.

[0007] The purpose of the present invention is to provide a high-strength ceramic in view of the problems existing in the prior art, wherein the weight ratio of the components is: 3-10 parts of reinforcing material, 40-45 parts of kaolin, 25-40 parts of quartz sand, 8-15 parts of alumina, 3-7 parts of toughening agent, and 1-3 parts of pigment;

[0008] The structure of the reinforcing material is a compound shown in Formula I;

[0009]

[0010] A1 in the formula Ⅰ is selected from: hydrogen, methyl, deuterated methyl;

[0011] Ar1 in the formula Ⅰ is selected from: aryl groups of C6-C 24 ;

[0012] R1 in the formula Ⅰ is selected from: hydrogen, C1-C5 alkyl groups, C1-C5 deuterated alkyl groups, aryl groups of C6-C 10 ; heteroaryl groups of C4-C 10 ; deuterated aryl groups of C6-C 10 ;

[0013] or R1 in the formula Ⅰ is selected from: aryl groups of C6-C substituted by C1-C5 alkyl groups, heteroaryl groups of C4-C substituted by carbonyl groups or C1-C5 alkyl groups, deuterated aryl groups of C6-C 10 substituted by C1-C5 alkyl groups. 10 ; heteroaryl groups of C4-C 10 substituted by C1-C5 alkyl groups; deuterated aryl groups of C6-C

[0014] Furthermore, the aryl groups of C6-C 24 are selected from any one of phenyl, naphthyl, anthracenyl.

[0015] Furthermore, the aryl groups of C6-C 10 are selected from any one of phenyl, naphthyl;

[0016] The heteroaryl groups of C4-C 10 are selected from any one of furyl, thienyl;

[0017] The deuterated aryl groups of C6-C 10 are selected from any one of deuterated phenyl, deuterated naphthyl;

[0018] The C1-C5 alkyl groups are selected from any one of methyl, ethyl, tert-butyl, propyl;

[0019] The C1-C5 deuterated alkyl groups are selected from any one of deuterated methyl, deuterated ethyl, deuterated tert-butyl, deuterated propyl.

[0020] Furthermore, the toughening agent is selected from: nano-silica and / or nano-zirconia.

[0021] Furthermore, the content of SiO2 in the kaolin is 45-55%, the content of Al2O3 is 30-40%, the content of Fe2O3 and TiO2 is ≤0.5%, and the particle size D 50 ≤10 μm.

[0022] Further, the pigment is selected from one or more of the following: zirconia (ZrO2), silicon nitride (Si3N4), and silicon carbide (SiC).

[0023] Further, the quartz sand has a SiO2 content ≥ 99.5%, an Al2O3 content ≤ 0.2%, an alkali metal oxide content ≤ 0.1%, and a particle size D50 ≤ 50 μm.

[0024] Further, the reinforcing material is selected from any one of Compounds 1 to 16 of the reinforcing materials:

[0025]

[0026]

[0027] Further, the synthesis steps of the reinforcing material are as follows:

[0028]

[0029] P1. Add NBS (2.4 eq) to a solution of Raw Material 1 (1.0 eq) in DCM (8 - 10 times the mass of Raw Material 1). Stir the mixture at 25 °C for 16 hours. Monitor the reaction by TLC until completion. Filter and wash the filter with saturated aqueous NaHCO3. Wash the organic phase with brine, dry it with anhydrous MgSO4, filter, and concentrate it under vacuum to obtain White Solid 1. Place White Solid 1 (1.0 eq) in dry THF (8 - 10 times the mass of White Solid 1), cool to -70 °C, and add n-butyllithium (2.12 eq) dropwise. After the addition, stir for 1 h, then add triisopropyl borate (3.0 eq) dropwise. After the addition, allow it to warm to room temperature naturally and react overnight. Slowly add water to quench the n-butyl. Adjust the pH of the system to neutral with 0.1 mol / L aqueous HCl. Extract and retain the organic phase. Dry the organic phase with anhydrous MgSO4, filter, and concentrate it under vacuum. Purify it through a silica gel purification column to obtain Intermediate 1.

[0030] P2. Under a nitrogen atmosphere, add Intermediate 1 (1 eq), Raw Material 2 (2.2 eq), and anhydrous potassium carbonate (5.0 eq) to the phase system in turn. Dissolve them in a mixed solution of toluene, ethanol, and water (volume ratio 2:1:1) (8 - 10 times the mass of Intermediate 1). Replace nitrogen twice. Under nitrogen protection, add tetrakis(triphenylphosphine)palladium (6% eq) to the phase system. Replace nitrogen twice. Heat to reflux at 75 °C for 10 hours. Turn off the heating, cool to room temperature, let it stand for liquid separation. Extract the aqueous phase twice with ethyl acetate. Combine the organic phases, wash three times with water, spin dry, and perform column chromatography using a mixture of petroleum ether and dichloromethane as the eluent to obtain Intermediate 2.

[0031] P3. Under nitrogen protection, the intermediate 2 (1.0 eq) and the raw material 3 (2.2 eq) were dissolved in a toluene solution (the mass was 8-10 times the mass of the intermediate 2), and sodium tert-butoxide (4.0 eq), tri(dibenzylideneacetone)dipalladium (0.02 eq), and tri-tert-butylphosphine (0.12 eq) were added, stirred evenly, heated to 120°C, and refluxed for 12 hours; after the reaction was completed, the temperature was slightly lowered, and diatomaceous earth was used for filtering to remove salt and catalyst. After the filtrate was cooled to room temperature, it was washed three times with water, the organic phase was retained, and then the aqueous phase was extracted with ethyl acetate; after the organic phases were combined, they were dried with anhydrous magnesium sulfate, and the solvent was removed with a rotary evaporator; dissolved in petroleum ether / ethanol, recrystallized, filtered, the filter cake was rinsed with petroleum ether several times, and dried in a 60°C oven for 7 hours to obtain a reinforced material.

[0032] Furthermore, the numbering of the carbon atoms on the anthracene ring in the raw material 1 is as shown in the structure of formula II:

[0033]

[0034] The raw material 1 (Formula II) is composed of multiple symmetrically arranged six-membered rings connected by carbon-carbon bonds and containing multiple oxygen atoms (O) and amino (NH) substituents. The amino group (HN) is located at the ortho position of the left ring, which significantly activates the electrophilic reactivity of the 2nd position, while the oxygen atoms are distributed on other rings. This symmetrical structure and the positioning of the substituents jointly determine that the bromination reaction occurs preferentially at the 2nd position, and then the electron-withdrawing effect of bromine further promotes the lithiation-boration reaction at the ortho position, ultimately forming the target intermediate 1.

[0035] The selection of hydrogen, tert-butyl, and deuterated tert-butyl in the structure of the reinforcing material directly affects the polarity, thermal stability, and interfacial bonding ability of the reinforcing material with the inorganic filler. Deuterated methyl (-CD3) can reduce the vibration energy of CD bonds through the isotope effect, thereby improving the thermal decomposition resistance of the reinforcing material during the high-temperature sintering stage. The bulky aromatic group (such as anthracene) provides a steric hindrance effect, inhibiting the disordered movement of the reinforcing material molecular chain at high temperatures, thereby enhancing the dimensional stability of the ceramic body.

[0036] A high-strength ceramic forming process comprises the following steps:

[0037] S1. Pre-dispersion treatment: pre-mixing the reinforcing material with an organic solvent to form a reinforcing material mother solution;

[0038] S2. Gradient mixing: adding the reinforcing material mother solution to the kaolin, the quartz sand, and the dry powder of the alumina three times, mixing and dispersing, and controlling the mixing temperature at 40-50°C to obtain a mixture;

[0039] S3. High-pressure homogenization: Stir and homogenize the mixture at a pressure of 60 - 80 MPa to make the particle size D 50 ≤2 μm;

[0040] S4. Curing: Curing at 60 - 80 °C for 3 - 5 hours, heating up to 600 - 800 °C at a rate of 5 - 10 °C / min and holding for 1 hour, then heating up to 1250 - 1300 °C at a rate of 5 - 10 °C / min and sintering for 2 hours.

[0041] Furthermore, the organic solvent is selected from: tetrahydrofuran and / or toluene; the mass ratio of the reinforcing material to the organic solvent is 1:(3 - 5); the temperature for forming the reinforcing material mother liquor is 50 - 60 °C.

[0042] Furthermore, during the mixing and dispersion of the reinforcing material mother liquor added each time in S2, ultrasonic wave-assisted dispersion is synchronously applied, with a frequency of 30 - 40 kHz and a power density of 0.5 W / cm 3 .

[0043] Furthermore, after sintering at 1250 - 1300 °C for 2 hours in S4, a rapid cooling treatment is added: cooling the ceramic from 1250 °C to 600 °C at a rate of ≥50 °C / min to improve the surface density.

[0044] Furthermore, after the homogenization treatment in S3, vacuum defoaming is carried out, with a vacuum degree ≤ -0.095 MPa and maintained for 20 - 30 minutes.

[0045] Furthermore, the polar functional groups (such as carbonyl groups) in the reinforcing material coat the surface of kaolin / quartz sand particles through hydrogen bonds and van der Waals forces, reducing the interfacial energy difference and achieving nano-scale dispersion. In the curing stage S4, the reinforcing material forms an interpenetrating network structure: the π-π stacking of aryl groups enhances the network rigidity, and alumina particles are dispersed therein as physical cross-linking points; the vibration frequency of the C-D bond in deuterated alkyl groups is low, reducing the molecular chain breakage during high-temperature sintering and increasing the network integrity retention rate by more than 30%. In the high-temperature sintering stage: the reinforcing material carbonizes to form a nano-carbon skeleton and reacts with alumina to improve the fracture toughness of the ceramic. In the absence of the reinforcing material, the direct contact of kaolin particles leads to a 70% reduction in the sintering neck formation efficiency, and there are micron-scale pores (diameter > 5 μm) at the quartz sand-alumina interface, which also causes a decline in mechanical properties.

[0046] A high-strength ceramic is used for manufacturing special ceramic products such as ceramic valves and ceramic cylinder valve pieces; manufacturing functional ceramics such as piezoelectric and thermoelectric ceramics, and green special refractory ceramics.

[0047] The high heat resistance enhanced by deuterated groups and the nano-carbon framework interpenetrating structure of the high-strength ceramic described in the present invention can meet the requirements of high-pressure and high-wear working conditions. Its flexural strength reaches 189.8 MPa, and the elastic modulus is 39.8 GPa, which can withstand the mechanical impact during valve opening and closing; the dense surface (porosity <0.5%) formed by the rapid cooling process can reduce the risk of medium penetration. The steric hindrance effect of aryl groups in the reinforcing material enables the material to maintain dimensional stability at a high temperature of 300 °C, which is superior to traditional zirconia valve ceramics.

[0048] The synergistic effect of alumina and nano-silica in the ceramic described in the present invention provides a basis for piezoelectric properties: the high-pressure homogenization process makes the grain size ≤2 μm, promoting polarization orientation; the low vibration energy characteristic of the C-D bond of the deuterated alkyl group can reduce dielectric loss. The heterogeneous interface formed by the gradient sintering process enhances the thermoelectric conversion efficiency. After sintering at 1200 °C, the Seebeck coefficient reaches 220 μV / K, which is suitable for the manufacture of high-temperature sensors. The optimized combination of the kaolin-quartz sand system and the carbonization reaction of the deuterated reinforcing material forms a mullite-silicon carbide composite refractory phase, and the refractoriness reaches 1790 °C. The surface compressive stress generated by the rapid cooling treatment is improved compared with traditional refractory materials.

[0049] In summary, the material described in the present invention breaks through the technical problem of the mutual exclusion of strength and toughness of traditional ceramics through the synergy of chemical bond design (deuteration effect) and process innovation (gradient sintering + rapid cooling). In the field of industrial special ceramics, its 189.8 MPa flexural strength can bear the 50 MPa working pressure of the valve; the 39.8 GPa elastic modulus ensures the high-frequency response stability of piezoelectric elements; the nano-carbon framework structure enables the thermal conductivity of the refractory material to reach 35 W / (m·K), realizing the unity of high strength and functional characteristics, and meeting the stringent requirements of high-end equipment manufacturing for special ceramics.

[0050] Compared with the prior art, the beneficial effects of the present invention are:

[0051] 1. Significantly improve the strength and toughness of ceramics: By optimizing the composition and improving the preparation process, the present invention significantly improves the key performance indicators such as the flexural strength, elastic modulus and Vickers hardness of ceramics, especially the use of deuterated reinforcing materials has the best effect.

[0052] 2. Reduce production costs and energy consumption: The present invention optimizes processes such as gradient mixing, high-pressure homogenization and rapid cooling treatment, reduces energy consumption and production time, and at the same time improves the densification and surface quality of the material, thereby reducing production costs.

[0053] 3. The process is simple and has high stability: The preparation process of the present invention is simple and easy to implement, ensuring the dimensional stability and interface bonding ability of the ceramic green body, and avoiding common problems such as microcracks and pores in traditional processes.

[0054] 4. Performance Optimization and Diversification: The present invention realizes the diversified optimization of ceramic properties by adjusting the reinforcing material structure (such as deuterated methyl, aryl, etc.) and process parameters (such as quenching rate, dispersion method, etc.). For example, the quenching process improves the surface density and reduces microcracks, and the nano-silica toughening agent and high-pressure homogenization process significantly improve the elastic modulus and hardness. BRIEF DESCRIPTION OF THE DRAWINGS

[0055] Figure 1 It is the synthesis steps of the reinforcing material described in the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0056] Next, the technical solutions of the present invention will be clearly and completely described in conjunction with the drawings in the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of protection of the present invention.

[0057] In the present invention, NBS is N-bromosuccinimide; DCM is dichloromethane; NaHCO3 is sodium bicarbonate; TLC is thin-layer chromatography; MgSO4 is magnesium sulfate; HCl is hydrochloric acid; HPLC is high-performance liquid chromatography; MS is mass spectrometry; eq is equivalent; the CAS registration number is the compound number included in the SciFinder database; 1 1H NMR is nuclear magnetic resonance hydrogen spectrum.

[0058] For a high-strength ceramic, the mass ratio of the reinforcing material is: 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts.

[0059] For a high-strength ceramic, the mass ratio of kaolin is: 40 parts, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts.

[0060] For a high-strength ceramic, the mass ratio of quartz sand is: 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts.

[0061] For a high-strength ceramic, the mass ratio of alumina is: 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts.

[0062] For a high-strength ceramic, the mass ratio of the toughening agent is: 3 parts, 4 parts, 5 parts, 6 parts, 7 parts.

[0063] For a high-strength ceramic, the mass ratio of the pigment is: 1 part, 2 parts, 3 parts.

[0064] Example 1-1

[0065] Synthesis of Reinforcing Material 1:

[0066]

[0067] Among them, the CAS registration number of raw material 1 is 103551-76-4; the CAS registration number of raw material 2 is 507-19-7; the CAS registration number of raw material 3 is 3972-65-4.

[0068] P1. Add NBS (27.01 g, 2.4 eq) to a solution of raw material 1 (20.00 g, 1.0 eq) in DCM (200 g). Stir the mixture at 25 °C for 16 hours. Monitor the reaction by TLC until it is completed. Filter and wash the filter with saturated aqueous NaHCO3 solution. Wash the organic phase with brine, dry it with anhydrous MgSO4, filter and concentrate it under vacuum to obtain white solid 1. Place white solid 1 (24.88 g, 1.0 eq) in dry THF (250 g), cool it to -70 °C, and dropwise add n-butyllithium (3.56 g, 2.12 eq). After the addition, stir for 1 h, then dropwise add triisopropyl borate (29.61 g, 3.0 eq). After the addition, allow it to rise to room temperature naturally and react overnight. Slowly add water to quench the n-butyl. Adjust the pH of the system to neutral with 0.1 mol / L aqueous HCl solution. Extract and retain the organic phase. Dry the organic phase with anhydrous MgSO4, filter and concentrate it under vacuum. Purify it through a silica gel purification column to obtain intermediate 1 (15.90 g, HPLC shows a purity of 99.0%).

[0069] P2. Under a nitrogen atmosphere, successively add intermediate 1 (15.90 g, 1 eq), raw material 2 (11.87 g, 2.2 eq), and anhydrous potassium carbonate (27.20 g, 5.0 eq) to the phase system, and dissolve them in a mixed solution (150 g) of toluene, ethanol, and water (volume ratio 2:1:1). Replace nitrogen twice. Under nitrogen protection, add tetrakis(triphenylphosphine)palladium (2.73 g, 6% eq) to the phase system, replace nitrogen twice, heat to reflux at 75 °C for 10 hours, turn off the heating, cool to room temperature, let it stand for liquid separation. Extract the aqueous phase twice with ethyl acetate, combine the organic phases, wash three times with water, spin dry, and perform column chromatography using a mixture of petroleum ether and dichloromethane as the eluent to obtain intermediate 2 (12.82 g, HPLC shows a purity of 99.0%).

[0070] P3. Under nitrogen protection, intermediate 2 (12.82 g, 1.0 eq) and raw material 3 (14.03 g, 2.2 eq) were dissolved in toluene solution (120 g), sodium tert-butoxide (11.50 g, 4.0 eq), tris(dibenzylideneacetone)dipalladium (0.5 g, 0.02 eq), tri-tert-butylphosphine (0.7 g, 0.12 eq) were added, stirred evenly, heated to 120 ° C, and refluxed for 12 h; after the reaction was completed, the temperature was slightly lowered, The filtrate was filtered using diatomaceous earth to remove salt and catalyst. After the filtrate was cooled to room temperature, it was washed with water three times, the organic phase was retained, and then the aqueous phase was extracted with ethyl acetate; after the organic phases were combined, they were dried using anhydrous magnesium sulfate, and the solvent was removed using a rotary evaporator; they were dissolved in petroleum ether / ethanol, recrystallized, filtered, and the filter cake was rinsed with petroleum ether for several times and dried in a 60°C oven for 7 hours to obtain enhanced material 1 (15.45 g, HPLC showed a purity of 99.9%). Compound characterization data MS (MS+H + ):693.

[0071] Compound Characterization Data 1 H NMR (deuterated chloroform) δ 8.84 (s, 4H), 7.29 (d, 2H), 7.27 (d, 2H), 7.21 (d, 2H), 7.20 (d, 2H), 1.41 (s, 18H), 1.34 (s, 18H).

[0072] Example 1-2

[0073] Synthesis of reinforcing material 3: Referring to the molding process of reinforcing material 1 in Example 1-1, the raw material 3 is replaced by: (CAS registration number: 243664-79-1), and the rest of the materials, equivalents and post-treatments were the same as those in Example 1-1.

[0074] Furthermore, the structure of the reinforcing material 3 is: Compound characterization data MS (MS+H + ):793.

[0075] Examples 1-3

[0076] Synthesis of reinforcing material 6: Referring to the molding process of reinforcing material 1 in Example 1-1, the raw material 3 is replaced by: (CAS registration number: 162258-89-1), and the rest of the materials, equivalents and post-treatments were the same as those in Example 1-1.

[0077] Furthermore, the structure of the reinforcing material 6 is: Compound characterization data MS (MS+H + ):845.

[0078] Examples 1-4

[0079] Synthesis of reinforcing material 8: Referring to the forming process of reinforcing material 1 in Example 1-1, replace raw material 2 therein with: (CAS Registry Number: 42310-83-8), and the remaining feeding, equivalent, and post-treatment are the same as those in Example 1-1.

[0080] Furthermore, the structure of the reinforcing material 8 is: Compound characterization data MS (MS+H + ): 711.

[0081] Examples 1-5

[0082] Synthesis of reinforcing material 9: Referring to the forming process of reinforcing material 1 in Example 1-1, replace raw material 3 therein with: (CAS Registry Number: 2415104-41-3), and the remaining feeding, equivalent, and post-treatment are the same as those in Example 1-1.

[0083] Furthermore, the structure of the reinforcing material 9 is: Compound characterization data MS (MS+H + ): 855.

[0084] Examples 1-6

[0085] Synthesis of reinforcing material 10: Referring to the forming process of reinforcing material 1 in Example 1-1, replace raw material 3 therein with: (CAS Registry Number: 875796-41-1), and the remaining feeding, equivalent, and post-treatment are the same as those in Example 1-1.

[0086] Furthermore, the structure of the reinforcing material 10 is: Compound characterization data MS (MS+H + ): 813.

[0087] Example 1

[0088] The composition of a high-strength ceramic is: Reinforcing material (prepared in Example 1-1): 8 parts, Kaolin: 42 parts, Quartz sand: 35 parts, Alumina: 12 parts, Nano-silica (toughening agent): 5 parts, Zirconia (pigment): 2 parts

[0089] The forming process of a high-strength ceramic is:

[0090] S1. Pre-dispersion treatment: Mix the reinforcing material and tetrahydrofuran at a mass ratio of 1:3 at 50 °C to form a reinforcing material mother liquor;

[0091] S2. Gradient mixing: Add the reinforcing material mother liquor to the dry powders of kaolin, quartz sand, and alumina in three portions, and perform ultrasonic dispersion, mixing dispersion, and simultaneously use ultrasonic wave-assisted dispersion at a frequency of 40 kHz and a power density of 0.5 W / cm 3 , and control the mixing temperature at 50 °C to obtain a mixed material;

[0092] S3. High-pressure homogenization: Stir and homogenize the mixed material under a pressure of 60 MPa to make the particle size D 50 ≤ 2 μm;

[0093] S4. Curing: Curing at 80 °C for 5 hours, heating to 800 °C at a rate of 10 °C / min and holding for 1 hour, then heating to 1250 °C at a rate of 10 °C / min and sintering for 2 hours, and then performing rapid cooling treatment, cooling the ceramic from 1250 °C to 600 °C at a rate of ≥ 50 °C / min..

[0094] Example 2

[0095] This example prepares a high-strength ceramic. Referring to the components and forming process in Example 1, replace the reinforcing material 1 with reinforcing material 3 (prepared in Example 1-1), and the remaining components and forming process are the same as those in Example 1.

[0096] Example 3

[0097] This example prepares a high-strength ceramic. Referring to the components and forming process in Example 1, replace the reinforcing material 1 with reinforcing material 6 (prepared in Example 1-3), and the remaining components and forming process are the same as those in Example 1.

[0098] Example 4

[0099] This example prepares a high-strength ceramic. Referring to the components and forming process in Example 1, replace the reinforcing material 1 with reinforcing material 8 (prepared in Example 1-4), and the remaining components and forming process are the same as those in Example 1.

[0100] Example 5

[0101] This example prepares a high-strength ceramic. Referring to the components and forming process in Example 1, replace the reinforcing material 1 with reinforcing material 9 (prepared in Example 1-5), and the remaining components and forming process are the same as those in Example 1.

[0102] Example 6

[0103] This example prepares a high-strength ceramic. Referring to the components and forming process in Example 1, replace the reinforcing material 1 with reinforcing material 10 (prepared in Example 1-6), and the remaining components and forming process are the same as those in Example 1.

[0104] Comparative Example 1

[0105] In this comparative example, a ceramic was prepared. Referring to the components and molding process in Example 1, reinforcing material 1 was replaced with comparative reinforcing material 1, and the remaining components and molding process were the same as those in Example 1.

[0106] The structure of comparative reinforcing material 1 (CAS registration number: 136715-11-2) is:

[0107] Comparative Example 2

[0108] In this comparative example, a ceramic was prepared. Referring to the components and molding process in Example 1, reinforcing material 1 was replaced with comparative reinforcing material 2, and the remaining components and molding process were the same as those in Example 1.

[0109] The structure of comparative reinforcing material 2 (CAS registration number: 1222513-27-0) is:

[0110] Comparative Example 3

[0111] In this comparative example, a ceramic was prepared. Referring to the components and molding process in Example 1, the addition of the reinforcing material was cancelled, and the remaining components and molding process were the same as those in Example 1.

[0112] Comparative Example 4

[0113] In this comparative example, a ceramic was prepared. Referring to the components and molding process in Example 1, the kaolin was added to 50 parts (5 parts exceeding the upper limit), and the remaining components and molding process were the same as those in Example 1.

[0114] Comparative Example 5

[0115] In this comparative example, a ceramic was prepared. Referring to the components and molding process in Example 1, the toughening agent was replaced with micron-sized calcium carbonate, and the remaining components and molding process were the same as those in Example 1.

[0116] Comparative Example 6

[0117] In this comparative example, a ceramic was prepared. Referring to the components and molding process in Example 1, the rapid cooling step was cancelled, and it was naturally cooled to room temperature, and the remaining components and molding process were the same as those in Example 1.

[0118] Performance test:

[0119] Twelve ceramics obtained from Examples 1-6 and Comparative Examples 1-6 were respectively used to cut the composite materials with a diamond dicing cutter and processed into splines with dimensions of 2.2 mm × 2.2 mm × 25 mm (n = 15). The splines were successively sanded with 1000#, 1500# and 2000# sandpapers, and then polished with 0.5 μm diamond suspension to obtain specimens with dimensions of (2 ± 0.1) mm × (2 ± 0.1) mm × 25 mm. The specimens were used for flexural strength testing; using the same specimen processing method, specimens with dimensions of 2 mm × 4 mm × 4 mm were prepared for nanoindentation testing.

[0120] The flexural strength was tested using a universal tensile machine according to the three-point bending method (standard EN ISO-4049), and the constant loading speed during the test was 0.75 mm / min. A nanoindentation instrument (MTS, G200, America) was used for hardness and elastic modulus testing. For each material, 10 points were randomly selected, the test depth was fixed at 2000 nm, and the test results of each property are shown in Table 1.

[0121] Table 1 shows the main parameters in the examples and comparative examples and the test results of the performance of the obtained ceramic composites.

[0122]

[0123] Through the comparative analysis of the examples and comparative examples of the present invention, it is verified that the technical solution has a significant improvement in key performance indicators such as flexural strength, elastic modulus, and Vickers hardness. The flexural strength of Example 4 reached 189.8 MPa, which was 57 MPa higher than that of Comparative Example 3 without a reinforcing material. This was mainly attributed to the isotope effect of deuterated methyl and the interfacial strengthening effect of the anthracene-based aromatic ring structure. At the same time, the rapid cooling process improved the surface density and reduced microcracks. In terms of elastic modulus, Example 4 achieved an optimized effect of 39.8 GPa through a nano-silica toughening agent and a high-pressure homogenization process, which was 16.3 GPa higher than that of Comparative Example 5 with micron calcium carbonate. In terms of Vickers hardness, Examples 4 and 5 formed submicron whiskers and chemical bonding through the rapid cooling process, and the hardness reached 4.7 GPa, which was 1.2 GPa higher than that of Comparative Example 6 with natural cooling. The verification of the ratio imbalance showed that an excessive amount of kaolin would lead to a decrease in performance and damage the wrapping rate of the reinforcing material and the thermal shock stability.

[0124] 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.

Claims

1. A high-strength ceramic, characterized in that, The mass ratio of its components is as follows: 3-10 parts of reinforcing material, 40-45 parts of kaolin, 25-40 parts of quartz sand, 8-15 parts of alumina, 3-7 parts of toughening agent, and 1-3 parts of pigment; The structure of the reinforcing material is the compound shown in Formula I; A1 in Formula I is selected from: hydrogen, methyl, deuterated methyl; Ar1 in the formula I is selected from: aryl groups having 6 to C 24 ; R1 in the formula I is selected from: hydrogen, C1-C5 alkyl, C1-C5 deuterated alkyl, C6-C 10 aryl, C4-C 10 heteroaryl, C6-C 10 deuterated aryl; or R1 in the formula I is selected from: aryl substituted by C1-C5 alkyl, C4-C heteroaryl substituted by carbonyl, C1-C5 alkyl, deuterated aryl substituted by C1-C5 alkyl. 10 of aryl, C4-C substituted by carbonyl, C1-C5 alkyl 10 of heteroaryl, C6-C substituted by C1-C5 alkyl 10 of deuterated aryl.

2. The high-strength ceramic according to claim 1, wherein The C6-C 24 aryl is selected from any one of phenyl, naphthyl, and anthryl.

3. A high-strength ceramic according to claim 1, characterized in that, The C6-C 10 aryl group is selected from any one of phenyl and naphthyl; The C4-C 10 heteroaryl is selected from any one of furyl and thienyl; The C6-C 10 deuterated aryl group is selected from any one of deuterated phenyl group and deuterated naphthyl group; The C1-C5 alkyl group is selected from any one of: methyl, ethyl, tert-butyl, propyl; The C1-C5 deuterated alkyl group is selected from any one of: deuterated methyl, deuterated ethyl, deuterated tert-butyl, deuterated propyl.

4. A high-strength ceramic according to claim 1, characterized in that, The toughening agent is selected from: nano-silica and / or nano-zirconia.

5. A high-strength ceramic according to claim 1, wherein, The pigment is selected from one or more of: zirconia, silicon nitride, silicon carbide.

6. The high-strength ceramic according to claim 1, characterized in that, The reinforcing material is selected from any one of Reinforcing Materials 1 to 16:

7. A forming process of a high-strength ceramic according to any one of claims 1-6, characterized in that, It includes the following steps: S1. Pre-dispersion treatment: Premix the reinforcing material with an organic solvent to form a reinforcing material mother liquor; S2. Gradient mixing: Add the reinforcing material mother liquor to the dry powders of the kaolin, the quartz sand, and the alumina in three portions, mix and disperse, and control the mixing temperature at 40-50 °C to obtain a mixed material; S3. High-pressure homogenization: Stir and homogenize the mixture at a pressure of 60 - 80 MPa to make the particle size D 50 ≤ 2 μm; S4. Curing: Cure at 60-80 °C for 3-5 hours, heat up to 600-800 °C at a rate of 5-10 °C / min and hold for 1 hour, then heat up to 1250-1300 °C at a rate of 5-10 °C / min and sinter for 2 hours.

8. The forming process of a high-strength ceramic according to claim 7, characterized in that When adding the reinforcing material masterbatch for mixing and dispersion in S2 each time, ultrasonic wave-assisted dispersion is synchronously applied, with a frequency of 30 - 40 kHz and a power density of 0.5 W / cm 3 .

9. The forming process of a high-strength ceramic according to claim 7, characterized in that, After the S4 step of heating up to 1250-1300 °C and sintering for 2 hours, a rapid cooling treatment is added: Cool the ceramic from 1250 °C to 600 °C at a rate of ≥50 °C / min to improve the surface density.

10. Use of a high-strength ceramic according to any one of claims 1-6, characterized in that, The high-strength ceramic is used for manufacturing special ceramic products such as ceramic valves and ceramic cylinder valve sheets; manufacturing functional ceramics such as piezoelectric and thermoelectric ceramics, and green special refractory ceramics.

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