Novel ceramic preparation method

Abstract

The invention provides a novel ceramic preparation method, and relates to the technical field of ceramic preparation. The preparation method of the novel ceramic specifically comprises the following steps: S1, electrolytic treatment; s2, washing and drying; s3, mixing and grafting; s4, washing and drying again; s5, mixing again; s6, model printing; s7, naturally stabilizing; s8, firing the ceramic; and S9, standing and cooling. According to the method, through multi-step optimization treatment, the comprehensive performance of the ceramic material is remarkably improved, and meanwhile, the method also shows obvious advantages in the aspects of energy and environmental benefits, so that the technology has wide development prospects in preparation and application of advanced ceramic materials.

Description

Technical Field

[0001] The invention relates to the technical field of ceramic preparation, in particular to a novel ceramic preparation method. Background Art

[0002] Ceramics are solid substances formed by a high-temperature sintering process of inorganic, non-metallic materials. Ceramic materials usually have the characteristics of high hardness, high heat resistance, corrosion resistance, low conductivity and excellent chemical stability. Common ceramic materials include alumina, silicon dioxide, silicon nitride and silicon carbide. Ceramics are widely used in daily life, industrial production and high-tech fields, such as tableware, building materials, electronic components, biomedical materials and aerospace materials.

[0003] The materials used in traditional ceramic preparation methods are relatively conventional materials with certain performance limitations. Ceramic materials prepared by traditional methods usually have low strength, especially under high temperature or high pressure conditions, which limits their use in high-performance applications. In terms of corrosion resistance, traditional ceramic materials have poor chemical stability in certain corrosive media (such as acids, alkalis, salt solutions, etc.), are prone to corrosion or degradation, and are difficult to surface treat, making it difficult to perform effective corrosion resistance treatment. In terms of functional stability, traditional ceramic materials usually only have a single property, such as high hardness or high heat resistance, but lack the combination of multiple functions, and their performance is prone to change in environments with high temperature and large humidity changes, resulting in decreased functional stability. Summary of the invention

[0004] In view of the deficiencies in the prior art, the present invention provides a novel ceramic preparation method, which solves the problem that the raw materials used in the traditional preparation method are relatively single and have certain limitations in function and quality.

[0005] To achieve the above objectives, the present invention is implemented by the following technical solutions: a new ceramic preparation method, specifically comprising the following steps:

[0006] S1. Electrolytic treatment

[0007] Sprinkle 1000g of clay raw material evenly on the bottom of the electrolytic cell, add 500ml of 0.1M NaCl solution to ensure that the clay is completely immersed, then connect the electrolytic cell to the power supply and perform electrolysis for 30 minutes;

[0008] S2. Washing and drying

[0009] After the electrolytic treatment, the clay was removed from the solution, washed three times with deionized water, and then dried at 60 °C for 24 h;

[0010] S3. Hybrid grafting

[0011] 50 g of silane coupling agent 3-aminopropyltriethoxysilane was mixed with 1000 g of dried clay particles and 500 ml of ethanol, and stirred for 1 hour to ensure that the silane coupling agent was fully grafted on the surface of the clay particles;

[0012] S4. Wash and dry again

[0013] The grafted clay particles were washed with deionized water for three times to remove excess silane coupling agent, and then dried;

[0014] S5. Mix again

[0015] Mix the dried clay particles with 200 ml of YHY-6 organic mineral ion element concentrate and stir for 2 hours to ensure uniform mixing;

[0016] S6. Model printing

[0017] Add 100 grams of magnetic ferrite particles Fe3O4 to the mixture, then put the mixture into a 3D printing device and print it according to the preset shape and size for 30 minutes;

[0018] S7. Natural stability

[0019] After 3D printing is completed, the molded part is placed at room temperature for 24 hours to allow it to stabilize naturally;

[0020] S8. Ceramic firing

[0021] 50 grams of nanocarbon material was evenly coated on the surface of the molded part to form a photothermal conversion layer, and then the molded part was placed in a firing device of a synchrotron radiation light source, and the power of the synchrotron radiation light source was adjusted to gradually increase to 1000 W within 20 minutes, and then the power of 1000 W was maintained for 30 minutes;

[0022] S9 Cooling

[0023] After firing, the molded part was taken out from the synchrotron radiation device, placed in a holding furnace, kept at 1000°C for 2 hours, and then naturally cooled to room temperature.

[0024] Preferably, the YHY-6 type organic mineral ion element concentrate contains a variety of organic components and mineral ion elements, among which Al 3+ 、Si 4+ Mg 2+ , Ca 2+ , Fe 3+ .

[0025] Preferably, during the synchrotron radiation firing process, an in-situ X-ray diffractometer and a Raman spectrometer can be used to monitor the structural changes and performance development of the material in real time.

[0026] Preferably, the method further comprises forming a biomineralization coating with self-repairing ability on the ceramic surface by using silicate bacteria Baciluspasteur ii through biomineralization treatment to improve the hardness and corrosion resistance of the material.

[0027] Preferably, in the model printing of step S6, a magnetic field with an intensity of 0.5 T needs to be applied during the printing process, with the direction being perpendicular to the printing plane.

[0028] Preferably, in the electrolysis treatment in step S1, the current is adjusted to 0.5A and the voltage is adjusted to 5V.

[0029] Preferably, the washing and drying in step S4 is performed again at 60° C. for 12 hours.

[0030] The present invention provides a novel ceramic preparation method, which has the following beneficial effects:

[0031] The present invention provides a novel ceramic preparation method. The electrolytic pretreatment step of the present invention improves the activity of the clay surface by electrolytically treating the clay raw material in an electrolytic cell, and enhances the binding force between the clay particles and the silane coupling agent added in the subsequent step. The improvement of the surface activity lays a foundation for the subsequent chemical modification and the enhancement of mechanical properties. Secondly, the addition of a variety of mineral ion element concentrates YHY-6 type concentrates further optimizes the mechanical strength and corrosion resistance of the ceramic material. These concentrates contain a variety of beneficial elements (such as Al 3+ 、Si 4+ Mg 2+ ), can combine with clay particles through chemical reactions, significantly enhancing the hardness, toughness and corrosion resistance of the material. In addition, magnetic ferrite particles Fe3O4 are introduced into the ceramic material through magnetic field guided molding technology. These particles form an orderly arranged microstructure under the action of the magnetic field, which not only enhances the magnetic properties of the material, but also improves its overall functional stability. The magnetic field guided molding technology can accurately control the distribution and orientation of the magnetic particles, so that the ceramic material exhibits excellent performance in magnetic applications. At the same time, the orderly arrangement of the magnetic particles also significantly improves the mechanical strength and durability of the material, making it perform better under high stress or complex environments.

[0032] The present invention provides a novel ceramic preparation method. The method of the present invention realizes low-temperature sintering of ceramic materials under the action of a synchrotron radiation light source by introducing photothermal conversion material nanocarbon materials. Traditional ceramic sintering usually needs to be carried out at high temperatures, while the present method utilizes the characteristics of photothermal conversion materials and can complete the sintering process at a lower temperature. This not only significantly reduces the energy consumption during the sintering process, but also reduces the carbon emissions caused by high temperatures, which is in line with the current global trend of green environmental protection and energy conservation and emission reduction. Under the action of photothermal conversion materials, ceramic materials can achieve a densification effect at a lower temperature, avoiding the high energy consumption and environmental burden brought by traditional high-temperature sintering. DETAILED DESCRIPTION

[0033] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0034] The embodiment of the present invention provides a novel ceramic preparation method, which specifically comprises the following steps:

[0035] S1. Electrolytic treatment

[0036] Sprinkle 1000g of clay raw material evenly on the bottom of the electrolytic cell, add 500ml of 0.1M NaCl solution to ensure that the clay is completely immersed, then connect the electrolytic cell to the power supply, adjust the current to 0.5A and the voltage to 5V, and perform electrolysis for 30 minutes;

[0037] S2. Washing and drying

[0038] After the electrolytic treatment, the clay was removed from the solution, washed three times with deionized water, and then dried at 60 °C for 24 h;

[0039] S3. Hybrid grafting

[0040] 50 g of silane coupling agent 3-aminopropyltriethoxysilane was mixed with 1000 g of dried clay particles and 500 ml of ethanol, and stirred for 1 hour to ensure that the silane coupling agent was fully grafted on the surface of the clay particles;

[0041] S4. Wash and dry again

[0042] The grafted clay particles were washed with deionized water three times to remove excess silane coupling agent and then dried at 60 °C for 12 h;

[0043] S5. Mix again

[0044] Mix the dried clay particles with 200 ml of YHY-6 organic mineral ion element concentrate and stir for 2 hours to ensure uniform mixing;

[0045] S6. Model printing

[0046] 100 grams of magnetic ferrite particles Fe3O4 were added to the mixture, and then the mixture was placed in a 3D printing device and printed according to the preset shape and size. During the printing process, a magnetic field with a strength of 0.5T was applied perpendicular to the printing plane for 30 minutes.

[0047] S7. Natural stability

[0048] After 3D printing is completed, the molded part is placed at room temperature for 24 hours to allow it to stabilize naturally;

[0049] S8. Ceramic firing

[0050] 50 grams of nanocarbon material was evenly coated on the surface of the molded part to form a photothermal conversion layer, and then the molded part was placed in a firing device of a synchrotron radiation light source, and the power of the synchrotron radiation light source was adjusted to gradually increase to 1000 W within 20 minutes, and then the power of 1000 W was maintained for 30 minutes;

[0051] S9 Cooling

[0052] After firing, the molded part was taken out from the synchrotron radiation device, placed in a holding furnace, kept at 1000°C for 2 hours, and then naturally cooled to room temperature.

[0053] YHY-6 organic mineral ion element concentrate contains a variety of organic components and mineral ion elements, including Al 3+ 、Si 4+ Mg 2+ , Ca 2+ , Fe 3+ These elements can significantly improve the mechanical strength and corrosion resistance of ceramic materials. During the synchrotron radiation firing process, the use of in-situ X-ray diffractometers and Raman spectrometers can monitor the structural changes and performance development of materials in real time, ensuring precise control and optimization of the firing process.

[0054] After the clay raw materials are pretreated by electrolysis, the surface activity is significantly improved, which helps to improve the bonding force between the clay particles and the YHY-6 concentrate in the subsequent steps. Through the magnetic field-guided molding, the magnetic ferrite particles form an orderly arranged structure inside the ceramic, which significantly improves the mechanical properties and functional stability of the molded parts. During the firing process, the use of nano-carbon materials, a photothermal conversion material, can achieve sintering of ceramic materials at a lower temperature, significantly reducing energy consumption and carbon emissions. Through biomineralization treatment, a layer of biomineralized coating with self-repairing ability is formed on the surface of the ceramic using silicate bacteria Bac illus pasteur ii, which improves the hardness and corrosion resistance of the material.

[0055] Biomineralization

[0056] raw material:

[0057] Silicate bacteria Bacillus pasteur ii: 10 g

[0058] Culture medium: 500 ml (containing 10 g urea, 1 g glucose, 0.1 g CaCl2·2H2O, 1 g NH4Cl, 0.5 g MgSO4·7H2O, 0.01 g FeSO4·7H2O, pH 7.0)

[0059] step:

[0060] The silicate bacteria were inoculated into 500 ml of the culture medium and cultured in a 37°C constant temperature shaker for 24 hours.

[0061] Place the fired ceramic piece into the culture medium, making sure its surface is completely immersed.

[0062] The ceramic pieces in the culture medium were placed in a constant temperature environment of 37°C and cultured for 7 days to allow the bacteria to form a biomineralized coating on the ceramic surface.

[0063] After the culture was completed, the ceramic pieces were taken out, washed three times with deionized water to remove excess bacteria and culture medium, and then dried at 60 °C for 12 h.

[0064] Electrolytic pretreatment improves surface activity:

[0065] The present invention significantly improves the activity of the clay surface through electrolytic treatment, thereby improving the bonding force between the clay particles and the subsequently added silane coupling agent and organic mineral ion element concentrate. The electrolytic treatment can also remove some impurities in the clay, purify the raw materials, and provide a purer substrate for subsequent steps.

[0066] Silane coupling agent grafting:

[0067] The grafting treatment of silane coupling agent 3-aminopropyltriethoxysilane (APTES) can enhance the interfacial bonding between clay particles and organic mineral ion element concentrate, thereby improving the mechanical properties and chemical stability of the final ceramic material. APTES grafting makes the surface of clay particles have certain chemically active groups, which is conducive to subsequent chemical reactions and coating formation.

[0068] Use of organic mineral ion element concentrate:

[0069] YHY-6 concentrate contains Al 3+ 、Si 4+ Mg 2+ , Ca 2+ , Fe 3+ Plasma elements, which can significantly improve the mechanical strength and corrosion resistance of ceramic materials. Through the stirring process, these ionic elements are evenly dispersed on the surface of the clay particles, thus obtaining a material with more consistent and stable properties.

[0070] Magnetic field guided molding:

[0071] The magnetic field applied during the 3D printing process causes the magnetic ferrite particles Fe3O4 to form an orderly arrangement inside the ceramic, significantly improving the mechanical properties and functional stability of the molded parts. Orderly arranged magnetic particles can enhance the magnetic properties of ceramic materials and expand their application in the field of magnetic materials.

[0072] Use of photothermal conversion materials:

[0073] The photothermal conversion layer of nanocarbon materials can realize the sintering of ceramic materials at a lower temperature, thereby significantly reducing energy consumption and carbon emissions. By firing with a synchrotron radiation light source, uniform heating can be achieved in a short time, ensuring the efficiency and uniformity of the sintering process.

[0074] Precise control of synchrotron radiation firing:

[0075] In-situ X-ray diffractometers and Raman spectrometers are used to monitor the structural changes and performance development of the material in real time, ensuring precise control and optimization during the firing process. Precise control of the sintering process can avoid temperature fluctuations and local overheating, and improve the sintering quality of the final ceramic material.

[0076] Biomineralization treatment:

[0077] Through biomineralization treatment, a layer of self-healing biomineralized coating is formed on the ceramic surface using silicate bacteria Bacillus pasteur ii, which improves the hardness and corrosion resistance of the material. Biomineralization treatment is an environmentally friendly method that does not require the use of harmful chemicals and meets the requirements of sustainable development. Biomineralized coating not only improves the hardness and corrosion resistance of the material, but also may give the ceramic material other biological functions, such as antibacterial properties and biocompatibility.

[0078] Through multiple processing steps, especially electrolytic pretreatment, silane coupling agent grafting, the use of organic mineral ion element concentrate and magnetic field guided molding, the mechanical strength of the final ceramic material is significantly improved. The addition of biomineralized coating and organic mineral ion elements effectively improves the corrosion resistance of ceramic materials and extends their service life. Magnetic field guided molding and the use of photothermal conversion materials ensure the functional stability and reliability of ceramic materials. The use of photothermal conversion materials reduces the temperature of the sintering process, thereby significantly reducing energy consumption. Due to the reduction in sintering temperature, carbon emissions are also reduced accordingly, meeting the requirements of green manufacturing.

[0079] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A novel ceramic preparation method, characterized in that: The specific steps include: S1. Electrolytic treatment Sprinkle 1000g of clay raw material evenly on the bottom of the electrolytic cell, add 500ml of 0.1M NaCl solution to ensure that the clay is completely immersed, then connect the electrolytic cell to the power supply and perform electrolysis for 30 minutes; S2. Washing and drying After the electrolytic treatment, the clay was removed from the solution, washed three times with deionized water, and then dried at 60 °C for 24 h; S3. Hybrid grafting 50 g of silane coupling agent 3-aminopropyltriethoxysilane was mixed with 1000 g of dried clay particles and 500 ml of ethanol, and stirred for 1 hour to ensure that the silane coupling agent was fully grafted on the surface of the clay particles; S4. Wash and dry again The grafted clay particles were washed with deionized water for three times to remove excess silane coupling agent, and then dried; S5. Mix again Mix the dried clay particles with 200 ml of YHY-6 organic mineral ion element concentrate and stir for 2 hours to ensure uniform mixing; S6. Model printing Add 100 grams of magnetic ferrite particles Fe3O4 to the mixture, then put the mixture into a 3D printing device and print it according to the preset shape and size for 30 minutes; S7. Natural stability After 3D printing is completed, the molded part is placed at room temperature for 24 hours to allow it to stabilize naturally; S8. Ceramic firing 50 grams of nanocarbon material was evenly coated on the surface of the molded part to form a photothermal conversion layer, and then the molded part was placed in a firing device of a synchrotron radiation light source, and the power of the synchrotron radiation light source was adjusted to gradually increase to 1000 W within 20 minutes, and then the power of 1000 W was maintained for 30 minutes; S9 Cooling After firing, the molded part was taken out from the synchrotron radiation device, placed in a holding furnace, kept at 1000°C for 2 hours, and then naturally cooled to room temperature.

2. A novel ceramic preparation method according to claim 1, characterized in that: The YHY-6 organic mineral ion element concentrate contains a variety of organic components and mineral ion elements, among which Al 3+ 、Si 4+ Mg 2+ , Ca 2+ , Fe 3+ .

3. A novel ceramic preparation method according to claim 1, characterized in that: During the synchrotron radiation firing process, the structural changes and performance development of the material can be monitored in real time using an in-situ X-ray diffractometer and a Raman spectrometer.

4. A novel ceramic preparation method according to claim 1, characterized in that: The method also includes forming a biomineralization coating with self-repairing ability on the ceramic surface by using silicate bacteria Bacillus pasteurii through biomineralization treatment to improve the hardness and corrosion resistance of the material.

5. A novel ceramic preparation method according to claim 1, characterized in that: In the step S6 of model printing, a magnetic field with a strength of 0.5 T needs to be applied during the printing process, with the direction perpendicular to the printing plane.

6. A novel ceramic preparation method according to claim 1, characterized in that: In the electrolysis treatment of step S1, the current is adjusted to 0.5A and the voltage is adjusted to 5V.

7. A novel ceramic preparation method according to claim 1, characterized in that: In the step S4, the washing and drying is performed again at 60° C. for 12 hours.