CN113929489A - Ceramic and preparation method thereof - Google Patents
Ceramic and preparation method thereof Download PDFInfo
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- CN113929489A CN113929489A CN202111230950.XA CN202111230950A CN113929489A CN 113929489 A CN113929489 A CN 113929489A CN 202111230950 A CN202111230950 A CN 202111230950A CN 113929489 A CN113929489 A CN 113929489A
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The embodiment of the invention relates to the technical field of ceramics, in particular to a ceramic and a preparation method thereof, wherein the ceramic comprises the following components in parts by weight: 55-75 parts of silicon carbide powder, 4 parts of boron carbide, 10-25 parts of iron oxide, 10 parts of binder and 1 part of dispersant; the silicon carbide powder comprises alpha-silicon carbide micro powder with the particle size of 0.7-1.3 microns and beta-silicon carbide micro powder with the particle size of 3-4 microns. Through the mode, the embodiment of the invention can improve the apparent porosity of the ceramic, improve the filtering effect and enable the ceramic to have good high-temperature mechanical property.
Description
Technical Field
The embodiment of the invention relates to the technical field of ceramics, in particular to a ceramic and a preparation method thereof.
Background
The porous ceramic material has wide application prospect in the modern industrial field, and is favorable for precise filtration and separation of various media, high-pressure gas exhaust silencing, gas separation, electrolytic diaphragm and the like.
The inventor of the present application finds in research that, in the existing porous ceramics, organic matter pore-forming, in-situ reaction pore-forming or foaming pore-forming is mostly adopted, a large amount of organic matter needs to be added in the preparation process, and although the resulting porosity is high, that is, the volume of pores accounts for a high percentage of the total volume, the apparent porosity is low, that is, the proportion of pore communication is low, and thus the filtration effect is poor.
Disclosure of Invention
In view of the above problems, embodiments of the present invention provide a ceramic and a method for preparing the same, so as to improve the apparent porosity of the ceramic, improve the filtering effect, and provide the ceramic with good high-temperature mechanical properties.
According to an aspect of an embodiment of the present invention, there is provided a ceramic, including, in parts by weight: 55-75 parts of silicon carbide powder, 4 parts of boron carbide, 10-25 parts of iron oxide, 10 parts of binder and 1 part of dispersant; the silicon carbide powder comprises alpha-silicon carbide micro powder with the particle size of 0.7-1.3 microns and beta-silicon carbide micro powder with the particle size of 3-4 microns.
In an alternative mode, the weight ratio of the alpha-silicon carbide micropowder to the beta-silicon carbide micropowder is 4: 1.
In an optional mode, the silicon carbide powder accounts for 55-70 parts by weight, and the ceramic further comprises 5 parts of epoxy resin.
In an alternative form, the boron carbide has a particle size of 2.5 microns.
In an optional mode, the particle size of the iron oxide is 30-50 nanometers.
In an alternative form, the binder comprises polyvinyl alcohol.
In an alternative form, the dispersant comprises polyethylene glycol.
According to another aspect of embodiments of the present invention, there is provided a method for preparing a ceramic, the method including: taking 55-75 parts by weight of silicon carbide powder, 4 parts by weight of boron carbide, 10-25 parts by weight of iron oxide, 10 parts by weight of binder and 1 part by weight of dispersant as raw materials, adding absolute ethyl alcohol, uniformly stirring and mixing, and performing ball milling to obtain slurry; granulating the slurry to obtain powder; carrying out compression molding on the powder to obtain a biscuit; heating at constant temperature to remove anhydrous ethanol and water in the biscuit to obtain dried biscuit; and sintering the dried biscuit for 14-17 hours at the temperature of 2100-2150 ℃ to obtain the ceramic.
In an optional mode, the slurry is subjected to spray granulation, and the temperature of an outlet during the spray granulation is 80-85 ℃.
In an alternative mode, the weight ratio of the raw material to the absolute ethyl alcohol is 1: 1.
According to the invention, 55-75 parts of silicon carbide powder, 4 parts of boron carbide, 10-25 parts of iron oxide, 10 parts of binder and 1 part of dispersant are adopted, wherein the silicon carbide powder comprises alpha-silicon carbide micro powder with the particle size of 0.7-1.3 microns and beta-silicon carbide micro powder with the particle size of 3-4 microns, so that the prepared ceramic has high apparent porosity, large specific surface area and strength meeting the application requirements.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
fig. 1 is a schematic flow chart of a ceramic preparation method according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
According to an aspect of an embodiment of the present invention, there is provided a ceramic, including, in parts by weight: 55-75 parts of silicon carbide powder, 4 parts of boron carbide, 10-25 parts of iron oxide, 10 parts of binder and 1 part of dispersant; the silicon carbide powder comprises alpha-silicon carbide micro powder with the particle size of 0.7-1.3 microns and beta-silicon carbide micro powder with the particle size of 3-4 microns, and the weight ratio of the alpha-silicon carbide micro powder to the beta-silicon carbide micro powder is 4: 1.
The boron carbide is used as a sintering aid, and specifically, the boron carbide can be dissolved in the silicon carbide in a solid solution manner, so that the interface energy of the silicon carbide is reduced, and the sintering process in the ceramic preparation process is promoted.
The iron oxide is used as a pore forming agent, and particularly, the iron oxide can react with silicon carbide at high temperature, and the reaction equation is as follows:
Fe2O3(l)+3SiC(s)→3Si(s)+2Fe(g)+3CO(g) (1)
SiC(s)→Si(g)+C(s) (2)
SiC(s)→Si(g)+SiC2(g) (3)
Si(g)+SiC(s)→Si2C(g) (4)
wherein, the equation (1) can be carried out at 1565 ℃, and the liquefied iron oxide reacts with the silicon carbide to generate Si gas, Fe gas and CO gas. At higher temperatures, part of the silicon carbide decomposes into Si gas and SiC as shown in equations (2) and (3)2A gas. The gasified Si in equation (2) and equation (3) also reacts with the SiC solid to produce gaseous Si2C, volatilizing. From this, we can see that after the iron oxide reacts with the silicon carbide, Si, Fe, CO and SiC are generated2And Si2C impurities are volatilized in a gas mode, so that the content of silicon carbide and iron oxide is reduced, pores are generated, and impurities except SiC in the prepared ceramic are volatilized in a gas mode, so that the purity of the ceramic is extremely high.
Because the silicon carbide powder comprises alpha-silicon carbide micro powder with the particle size of 0.7-1.3 microns and beta-silicon carbide micro powder with the particle size of 3-4 microns, in the sintering process, the alpha-silicon carbide is used as a crystal mother, the beta-silicon carbide generates phase change and is converted into the beta-silicon carbide micro powder, a dissolving-redeposition process is carried out simultaneously, the generated alpha-silicon carbide is deposited on the original alpha-silicon carbide crystal mother, the particle growth is anisotropic, a Core/Shell structure is generated through the dissolving and reprecipitation process, the beta-silicon carbide phagocytoses the alpha-silicon carbide and grows along a specific crystal orientation, the formed crystal has a better length-diameter ratio, and the strengthening and toughening effects can be achieved through crystal grain bridging.
In addition, for the silicon carbide particle systems with two particle sizes, when the size ratio of coarse particles to fine particles is more than or equal to 3 (the particle size of alpha-silicon carbide adopted in the experiment is 1 μm, the particle size of beta-silicon carbide is 3.5 μm, and the size ratio is 3.5), the grading effect of the system is most obvious, and the free bulk density of the system is high, so that the green density of the sample after compression molding is high, and the method is favorable for obtaining a more compact sample after sintering.
The iron oxide is low in price, the pore is formed by adopting the oxidant, the raw material cost of the ceramic is favorably reduced, impurities except SiC in the prepared ceramic are volatilized in a gas form, the purity of the ceramic is extremely high, and the ceramic is ensured to have good structural strength.
According to the invention, 55-75 parts of silicon carbide powder, 4 parts of boron carbide, 10-25 parts of iron oxide, 10 parts of binder and 1 part of dispersant are adopted, wherein the silicon carbide powder comprises alpha-silicon carbide micro powder with the particle size of 0.7-1.3 microns and beta-silicon carbide micro powder with the particle size of 3-4 microns, so that the prepared ceramic has high apparent porosity, large specific surface area and strength meeting the application requirements.
In order to ensure the structural strength of the ceramic, the application further provides an implementation mode, and specifically, the weight ratio of the alpha-silicon carbide micro powder to the beta-silicon carbide micro powder is 4: 1.
Through experimental research, the inventor of the application finds that when the weight ratio of the alpha-silicon carbide micro powder to the beta-silicon carbide micro powder is 4:1, the alpha-silicon carbide micro powder with smaller particle size can be effectively filled in the pores generated after the reaction of the beta-silicon carbide micro powder and the ferric oxide, so that the structural strength of the ceramic is ensured to be good.
In order to promote the diffusion of the boron carbide, the application further provides an implementation mode, specifically, the silicon carbide powder is 55-70 parts by weight, and the ceramic further comprises 5 parts by weight of epoxy resin.
The epoxy resin is used as a carbon source, the epoxy resin is added with carbon, the carbon is added to facilitate the removal of silicon dioxide on the surface of the silicon carbide powder, the surface energy of the silicon carbide powder is improved, so that the activity of the silicon carbide powder is improved, the diffusion of boron carbide is promoted, and the progress of a sintering process in the preparation process of the ceramic is promoted by promoting the diffusion of the boron carbide.
According to some embodiments of the present application, the boron carbide has a particle size of 2.5 microns.
By controlling the particle size of the boron carbide to be 2.5 microns, the boron carbide is facilitated to be dissolved in the silicon carbide powder in a solid manner so as to reduce the interfacial energy of the silicon carbide powder, thereby further promoting the sintering process.
According to some embodiments of the present application, the iron oxide has a particle size of 30 to 50 nm.
The particle size of the iron oxide is controlled to be 30-50 nanometers, so that the iron oxide and the silicon carbide powder can fully react, the porosity and apparent porosity of the prepared ceramic are improved, and the filtering effect is improved.
In order to improve the bonding effect of the ceramic raw material, the application further provides an embodiment, and specifically, the bonding agent comprises polyvinyl alcohol.
Polyvinyl alcohol is an organic compound of the formula [ C ]2H4O]nThe appearance is white flaky, flocculent or powdery solid and is tasteless. Is soluble in water (above 95 deg.C), slightly soluble in dimethyl sulfoxide, and insoluble in gasoline, kerosene, vegetable oil, benzene, toluene, dichloroethane, carbon tetrachloride, acetone, ethyl acetate, methanol, and ethylene glycol. Polyvinyl alcohol is an important chemical raw material, and is used for manufacturing polyvinyl acetal, gasoline-resistant pipelines, vinylon, fabric treating agents, emulsifiers, paper coatings, adhesives, glue and the like. Polyvinyl alcohol is a water-soluble high molecular polymer, is prepared by polymerizing and alcoholyzing vinyl acetate, and has unique performance, good adhesion, film forming property, oil resistance and colloid protection.
In order to improve the dispersion effect of the ceramic raw material, the application further provides an embodiment, and specifically, the dispersant comprises polyethylene glycol.
Polyethylene glycol is a high molecular polymer with the chemical formula HO (CH)2CH2O)nH, no irritation, slightly bitter taste, good tasteWater-solubility and good compatibility with a plurality of organic components. Has excellent lubricity, moisture retention, dispersibility and adhesiveness, can be used as an antistatic agent, a softening agent and the like, and has extremely wide application in industries such as cosmetics, pharmacy, chemical fibers, rubber, plastics, papermaking, paint, electroplating, pesticides, metal processing, food processing and the like.
According to another aspect of the embodiments of the present invention, there is provided a method for preparing a ceramic, specifically referring to fig. 1, which illustrates a flow of the method for preparing a ceramic, the method comprising:
s10: taking 55-75 parts by weight of silicon carbide powder, 4 parts by weight of boron carbide, 10-25 parts by weight of iron oxide, 10 parts by weight of binder and 1 part by weight of dispersant as raw materials, adding absolute ethyl alcohol, uniformly stirring and mixing, and performing ball milling to obtain slurry;
specifically, silicon carbide grinding balls can be used for ball milling, the weight ratio of the silicon carbide grinding balls to the raw materials can be 12:10, and the ball milling time is 6-8 hours, so that the high efficiency and the sufficient ball milling are facilitated.
S20: granulating the slurry to obtain powder;
the granulation can adopt agglomeration type granulation, extrusion type granulation, spray granulation and other modes;
specifically, the agglomeration granulation is to agglomerate slurry in motion under the action of rotation, vibration, stirring and the like; the extrusion type granulation is a method for preparing the slurry into a cylindrical shape, a spherical shape or a sheet shape by adopting mechanical processing such as extrusion, roller extrusion or pressing, and the like, and the spray granulation is a method for directly granulating after concentrating solid in the slurry;
s30: compression molding the powder to obtain a biscuit;
the powder can be molded by dry pressing equipment, and particularly, the dry pressing refers to a blank forming method which is commonly used in ceramic production. Adding a small amount of adhesive into powder for granulation, then loading the powder into a die, pressurizing the powder on a press machine to enable the powder particles to approach each other in the die and firmly combine the powder particles by internal friction force to form a blank body with a certain shape, wherein the pressure of dry pressing is generally controlled to be 20-40 Mpa, and the size of the formed biscuit is controlled by adjusting the size of the die;
s40: heating at constant temperature to remove anhydrous ethanol and water in the biscuit to obtain dried biscuit;
specifically, the constant temperature heating temperature is generally controlled within 100-150 ℃, and the heating time is 80-150 minutes;
s50: sintering the dried biscuit for 14-17 hours at the temperature of 2100-2150 ℃ to obtain ceramic;
and (2) placing the dried biscuit in a sintering device, and then starting to heat up the sintering device, wherein in order to facilitate the full and effective sintering, the heating speed is controlled to be 2-3 ℃/min in the process from room temperature to 900 ℃, the heating speed is controlled to be 4-6 ℃/min in the process from 900 ℃ to 1700 ℃, and the heating speed is controlled to be 3 ℃/min in the process from 1700 ℃ to 2150 ℃.
In order to achieve a suitable and uniform particle size of the granulated powder, the present application further proposes an embodiment, specifically, step S20 includes:
and (3) carrying out spray granulation on the slurry, wherein the temperature of an outlet is 80-85 ℃ during spray granulation.
The slurry is granulated through the atomizer, specifically, the slurry is dispersed into fog drops through the atomizer, powder with uniform and proper particle size is obtained through a mode that hot air directly contacts the fog drops, the temperature of an outlet is controlled to be 80-85 ℃, the powder with the particle size of 20-40 micrometers can be smoothly obtained, and the problem that the subsequent compression molding cannot be carried out due to the fact that the particle size of the powder is not proper is avoided.
In order to ensure that the components in the raw materials are uniformly and fully mixed, the application further provides an implementation mode, and specifically, the weight ratio of the raw materials to the absolute ethyl alcohol is 1: 1.
By adding the same amount of absolute ethyl alcohol into the raw materials, the components in the raw materials can be fully mixed in the absolute ethyl alcohol, and the smooth obtaining of slurry after ball milling can be ensured.
In order to more intuitively embody the effects of the ceramics obtained in the present application, the following description will be given by way of specific examples of the method for preparing ceramics.
Example 1:
taking 60 parts by weight of alpha-silicon carbide micro powder, 15 parts by weight of beta-silicon carbide micro powder, 4 parts by weight of boron carbide, 10 parts by weight of iron oxide, 10 parts by weight of polyvinyl alcohol and 1 part by weight of polyethylene glycol as raw materials, adding absolute ethyl alcohol according to a weight ratio of 1:1, uniformly stirring and mixing, and carrying out ball milling on the mixture by using silicon carbide grinding balls according to a weight ratio of 12:10 of the raw materials for 8 hours to obtain slurry;
carrying out spray granulation on the slurry, wherein the outlet temperature is 85 ℃ when the spray granulation is carried out, so as to obtain powder;
dry-pressing the powder material with dry-pressing equipment to obtain the product with the size of 50 × 50 × 4.5mm3The biscuit of (1);
heating the biscuit at the constant temperature of 120 ℃ for 100 minutes to discharge absolute ethyl alcohol and moisture in the biscuit to obtain a dried biscuit;
sintering the dried biscuit for 15.5 hours at the temperature of 2115 ℃ to obtain the ceramic, wherein the temperature rise speed of sintering equipment is controlled as follows: the room temperature is 900 ℃ below zero, the heating rate is 2.5 ℃/min, 900 plus 1700 ℃, the heating rate is 5 ℃/min, 1700 plus 2115 ℃, and the heating rate is 3 ℃/min.
Example 2:
taking 56 parts by weight of alpha-silicon carbide micro powder, 14 parts by weight of beta-silicon carbide micro powder, 4 parts by weight of boron carbide, 15 parts by weight of ferric oxide, 10 parts by weight of polyvinyl alcohol and 1 part by weight of polyethylene glycol as raw materials, adding absolute ethyl alcohol according to a weight ratio of 1:1, uniformly stirring and mixing, and carrying out ball milling on the mixture by using silicon carbide grinding balls according to a weight ratio of 12:10 of the raw materials for 8 hours to obtain slurry;
carrying out spray granulation on the slurry, wherein the outlet temperature is 85 ℃ when the spray granulation is carried out, so as to obtain powder;
dry-pressing the powder material with dry-pressing equipment to obtain the product with the size of 50 × 50 × 4.5mm3The biscuit of (1);
heating the biscuit at the constant temperature of 120 ℃ for 100 minutes to discharge absolute ethyl alcohol and moisture in the biscuit to obtain a dried biscuit;
sintering the dried biscuit for 15.5 hours at the temperature of 2115 ℃ to obtain the ceramic, wherein the temperature rise speed of sintering equipment is controlled as follows: the room temperature is 900 ℃ below zero, the heating rate is 2.5 ℃/min, 900 plus 1700 ℃, the heating rate is 5 ℃/min, 1700 plus 2115 ℃, and the heating rate is 3 ℃/min.
Example 3:
taking 52 parts by weight of alpha-silicon carbide micro powder, 13 parts by weight of beta-silicon carbide micro powder, 4 parts by weight of boron carbide, 20 parts by weight of ferric oxide, 10 parts by weight of polyvinyl alcohol and 1 part by weight of polyethylene glycol as raw materials, adding absolute ethyl alcohol according to a weight ratio of 1:1, uniformly stirring and mixing, and carrying out ball milling on the mixture by using silicon carbide grinding balls according to a weight ratio of 12:10 of the raw materials for 8 hours to obtain slurry;
carrying out spray granulation on the slurry, wherein the outlet temperature is 85 ℃ when the spray granulation is carried out, so as to obtain powder;
dry-pressing the powder material with dry-pressing equipment to obtain the product with the size of 50 × 50 × 4.5mm3The biscuit of (1);
heating the biscuit at the constant temperature of 120 ℃ for 100 minutes to discharge absolute ethyl alcohol and moisture in the biscuit to obtain a dried biscuit;
sintering the dried biscuit for 15.5 hours at the temperature of 2115 ℃ to obtain the ceramic, wherein the temperature rise speed of sintering equipment is controlled as follows: the room temperature is 900 ℃ below zero, the heating rate is 2.5 ℃/min, 900 plus 1700 ℃, the heating rate is 5 ℃/min, 1700 plus 2115 ℃, and the heating rate is 3 ℃/min.
Example 4:
according to parts by weight, 48 parts of alpha-silicon carbide micro powder, 12 parts of beta-silicon carbide micro powder, 4 parts of boron carbide, 25 parts of iron oxide, 10 parts of polyvinyl alcohol and 1 part of polyethylene glycol are taken as raw materials, absolute ethyl alcohol is added according to the weight ratio of 1:1, the raw materials are uniformly stirred and mixed, and the raw materials and silicon carbide grinding balls with the weight ratio of 12:10 are subjected to ball milling for 8 hours to obtain slurry;
carrying out spray granulation on the slurry, wherein the outlet temperature is 85 ℃ when the spray granulation is carried out, so as to obtain powder;
dry-pressing the powder material with dry-pressing equipment to obtain the product with the size of 50 × 50 × 4.5mm3The biscuit of (1);
heating the biscuit at the constant temperature of 120 ℃ for 100 minutes to discharge absolute ethyl alcohol and moisture in the biscuit to obtain a dried biscuit;
sintering the dried biscuit for 15.5 hours at the temperature of 2115 ℃ to obtain the ceramic, wherein the temperature rise speed of sintering equipment is controlled as follows: the room temperature is 900 ℃ below zero, the heating rate is 2.5 ℃/min, 900 plus 1700 ℃, the heating rate is 5 ℃/min, 1700 plus 2115 ℃, and the heating rate is 3 ℃/min.
Example 5:
taking 56 parts by weight of alpha-silicon carbide micro powder, 14 parts by weight of beta-silicon carbide micro powder, 4 parts by weight of boron carbide, 10 parts by weight of ferric oxide, 10 parts by weight of polyvinyl alcohol, 1 part by weight of polyethylene glycol and 5 parts by weight of epoxy resin as raw materials, adding absolute ethyl alcohol according to a weight ratio of 1:1, uniformly stirring and mixing, and carrying out ball milling on the mixture by using silicon carbide grinding balls according to a weight ratio of 12:10 of the raw materials for 8 hours to obtain slurry;
carrying out spray granulation on the slurry, wherein the outlet temperature is 85 ℃ when the spray granulation is carried out, so as to obtain powder;
dry-pressing the powder material with dry-pressing equipment to obtain the product with the size of 50 × 50 × 4.5mm3The biscuit of (1);
heating the biscuit at the constant temperature of 120 ℃ for 100 minutes to discharge absolute ethyl alcohol and moisture in the biscuit to obtain a dried biscuit;
sintering the dried biscuit for 15.5 hours at the temperature of 2115 ℃ to obtain the ceramic, wherein the temperature rise speed of sintering equipment is controlled as follows: the room temperature is 900 ℃ below zero, the heating rate is 2.5 ℃/min, 900 plus 1700 ℃, the heating rate is 5 ℃/min, 1700 plus 2115 ℃, and the heating rate is 3 ℃/min.
Example 6:
taking 52 parts by weight of alpha-silicon carbide micro powder, 13 parts by weight of beta-silicon carbide micro powder, 4 parts by weight of boron carbide, 15 parts by weight of ferric oxide, 10 parts by weight of polyvinyl alcohol, 1 part by weight of polyethylene glycol and 5 parts by weight of epoxy resin as raw materials, adding absolute ethyl alcohol according to a weight ratio of 1:1, uniformly stirring and mixing, and carrying out ball milling on the mixture by using silicon carbide grinding balls according to a weight ratio of 12:10 of the raw materials for 8 hours to obtain slurry;
carrying out spray granulation on the slurry, wherein the outlet temperature is 85 ℃ when the spray granulation is carried out, so as to obtain powder;
dry-pressing the powder material with dry-pressing equipment to obtain the product with the size of 50 × 50 × 4.5mm3The biscuit of (1);
heating the biscuit at the constant temperature of 120 ℃ for 100 minutes to discharge absolute ethyl alcohol and moisture in the biscuit to obtain a dried biscuit;
sintering the dried biscuit for 15.5 hours at the temperature of 2115 ℃ to obtain the ceramic, wherein the temperature rise speed of sintering equipment is controlled as follows: the room temperature is 900 ℃ below zero, the heating rate is 2.5 ℃/min, 900 plus 1700 ℃, the heating rate is 5 ℃/min, 1700 plus 2115 ℃, and the heating rate is 3 ℃/min.
Example 7:
taking 48 parts by weight of alpha-silicon carbide micro powder, 12 parts by weight of beta-silicon carbide micro powder, 4 parts by weight of boron carbide, 20 parts by weight of ferric oxide, 10 parts by weight of polyvinyl alcohol, 1 part by weight of polyethylene glycol and 5 parts by weight of epoxy resin as raw materials, adding absolute ethyl alcohol according to a weight ratio of 1:1, uniformly stirring and mixing, and carrying out ball milling on the mixture by using silicon carbide grinding balls according to a weight ratio of 12:10 of the raw materials for 8 hours to obtain slurry;
carrying out spray granulation on the slurry, wherein the outlet temperature is 85 ℃ when the spray granulation is carried out, so as to obtain powder;
dry-pressing the powder material with dry-pressing equipment to obtain the product with the size of 50 × 50 × 4.5mm3The biscuit of (1);
heating the biscuit at the constant temperature of 120 ℃ for 100 minutes to discharge absolute ethyl alcohol and moisture in the biscuit to obtain a dried biscuit;
sintering the dried biscuit for 15.5 hours at the temperature of 2115 ℃ to obtain the ceramic, wherein the temperature rise speed of sintering equipment is controlled as follows: the room temperature is 900 ℃ below zero, the heating rate is 2.5 ℃/min, 900 plus 1700 ℃, the heating rate is 5 ℃/min, 1700 plus 2115 ℃, and the heating rate is 3 ℃/min.
Example 8:
taking 44 parts by weight of alpha-silicon carbide micro powder, 11 parts by weight of beta-silicon carbide micro powder, 4 parts by weight of boron carbide, 25 parts by weight of ferric oxide, 10 parts by weight of polyvinyl alcohol, 1 part by weight of polyethylene glycol and 5 parts by weight of epoxy resin as raw materials, adding absolute ethyl alcohol according to a weight ratio of 1:1, uniformly stirring and mixing, and carrying out ball milling on the mixture by using silicon carbide grinding balls according to a weight ratio of 12:10 of the raw materials for 8 hours to obtain slurry;
carrying out spray granulation on the slurry, wherein the outlet temperature is 85 ℃ when the spray granulation is carried out, so as to obtain powder;
dry-pressing the powder material with dry-pressing equipment to obtain the product with the size of 50 × 50 × 4.5mm3The biscuit of (1);
heating the biscuit at the constant temperature of 120 ℃ for 100 minutes to discharge absolute ethyl alcohol and moisture in the biscuit to obtain a dried biscuit;
sintering the dried biscuit for 15.5 hours at the temperature of 2115 ℃ to obtain the ceramic, wherein the temperature rise speed of sintering equipment is controlled as follows: the room temperature is 900 ℃ below zero, the heating rate is 2.5 ℃/min, 900 plus 1700 ℃, the heating rate is 5 ℃/min, 1700 plus 2115 ℃, and the heating rate is 3 ℃/min.
The components in examples 1-8 are as follows in parts by weight:
TABLE 1
The microstructures of the ceramics prepared in examples 1 to 8 were uniform by microscopic observation, and the following conclusions were drawn by performing pore size, porosity, skeleton density and mechanical strength tests on the ceramics prepared in examples 1 to 8:
TABLE 2
According to the test data obtained in the examples 1-4 in the table 2, when no epoxy resin is added in the raw materials, the prepared ceramic can be ensured to have the pore diameter of 2.3-3.0 μm, the porosity of 29-41%, the apparent porosity of 27-37% and the skeleton density of 2.15-2.32 g/ml, meanwhile, the mechanical strength can reach 35-55 Mpa, and the mechanical strength can still reach 22-40 Mpa after high-temperature treatment at 800 ℃, so that the application strength requirement of common ceramics is met. Since porosity is an important index parameter when ceramics are used for filtration, porosity is inversely proportional to skeleton density, and the size of skeleton density directly affects mechanical strength of ceramics, it is preferable to prepare ceramics from 52 parts of α -silicon carbide fine powder, 13 parts of β -silicon carbide fine powder, 4 parts of boron carbide, 20 parts of iron oxide, 10 parts of polyvinyl alcohol and 1 part of polyethylene glycol as raw materials in order to achieve both porosity and mechanical strength of ceramics.
By comparing the test data obtained in the examples 5 to 8 in the table 2 with the test data obtained in the examples 1 to 4, it can be seen that the addition of 5 parts of epoxy resin to the raw materials is beneficial to further improving the mechanical strength of the ceramic, which can reach 50 to 65Mpa, and is also beneficial to fully improving the mechanical strength of the ceramic after high-temperature treatment at 800 ℃, which can reach 47 to 60Mpa, and simultaneously, the influence on the porosity and the apparent porosity is ensured to be small, so that the ceramic still has a good filtering effect. In order to satisfy the porosity requirement and the mechanical strength requirement when the ceramic is used for microfiltration and separation of various media, it is preferable to prepare the ceramic from 44 parts of fine α -silicon carbide powder, 11 parts of fine β -silicon carbide powder, 4 parts of boron carbide, 25 parts of iron oxide, 10 parts of polyvinyl alcohol, 1 part of polyethylene glycol, and 5 parts of epoxy resin as raw materials.
It is to be noted that technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which embodiments of the present invention belong, unless otherwise specified.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description. In particular, the technical features mentioned in the embodiments can be combined in any way as long as there is no structural conflict. It is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. A ceramic is characterized by comprising the following components in parts by weight: 55-75 parts of silicon carbide powder, 4 parts of boron carbide, 10-25 parts of iron oxide, 10 parts of binder and 1 part of dispersant;
the silicon carbide powder comprises alpha-silicon carbide micro powder with the particle size of 0.7-1.3 microns and beta-silicon carbide micro powder with the particle size of 3-4 microns.
2. The ceramic of claim 1, wherein the weight ratio of the alpha-silicon carbide micropowder to the beta-silicon carbide micropowder is 4: 1.
3. The ceramic according to claim 1, wherein the silicon carbide powder is 55-70 parts by weight, and the ceramic further comprises 5 parts by weight of epoxy resin.
4. The ceramic of claim 1, wherein the boron carbide has a particle size of 2.5 microns.
5. The ceramic according to claim 1, wherein the iron oxide has a particle size of 30 to 50 nm.
6. The ceramic of claim 1, wherein the binder comprises polyvinyl alcohol.
7. The ceramic of claim 1, wherein the dispersant comprises polyethylene glycol.
8. A method for preparing a ceramic, for preparing a ceramic according to any one of claims 1 to 7, the method comprising:
taking 55-75 parts by weight of silicon carbide powder, 4 parts by weight of boron carbide, 10-25 parts by weight of iron oxide, 10 parts by weight of binder and 1 part by weight of dispersant as raw materials, adding absolute ethyl alcohol, uniformly stirring and mixing, and performing ball milling to obtain slurry;
granulating the slurry to obtain powder;
carrying out compression molding on the powder to obtain a biscuit;
heating at constant temperature to remove anhydrous ethanol and water in the biscuit to obtain dried biscuit;
and sintering the dried biscuit for 14-17 hours at the temperature of 2100-2150 ℃ to obtain the ceramic.
9. The method for producing a ceramic according to claim 8, wherein the slurry is subjected to spray granulation, and the temperature of an outlet during the spray granulation is 80 to 85 ℃.
10. The method of claim 8, wherein the weight ratio of the feedstock to the absolute ethanol is 1: 1.
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Effective date of registration: 20231229 Address after: 411300 Fifth Floor of Pioneering Building, Shaoshan High-tech Industrial Development Zone, Xiangtan City, Hunan Province Patentee after: Hunan Dingyi New Material Co.,Ltd. Address before: 411105 No.27 yanggutang, Yuhu District, Xiangtan City, Hunan Province Patentee before: XIANGTAN University |