CN114195547A - High-strength porous silicon carbide ceramic material and preparation method thereof - Google Patents
High-strength porous silicon carbide ceramic material and preparation method thereof Download PDFInfo
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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
- C04B38/0615—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 the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
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- 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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Abstract
The invention discloses a high-strength porous silicon carbide ceramic material and a preparation method thereof, belongs to the technical field of functional materials, and aims at solving the problems that the existing secondary slurry coating process cannot eliminate holes and the strength is limited. According to the high-strength porous silicon carbide ceramic material and the preparation method thereof, the silicon powder in the first layer of slurry and the residual carbon generated by cracking of the polyurethane pore ribs are subjected to reactive sintering, so that the hollow structure of the pore ribs is reduced or even eliminated, secondary slurry dipping can be performed before sintering, and the mechanical strength and the thermal shock resistance of the high-strength porous silicon carbide ceramic material are further improved. Compared with the traditional secondary slurry coating process, the method can effectively eliminate or reduce holes of the porous silicon carbide ceramic material hole ribs and improve the density of the porous silicon carbide ceramic hole ribs; compared with siliconizing treatment, the method does not need secondary high-temperature sintering, has extremely low residual silicon content, and fundamentally solves the problem of low strength of the porous silicon carbide ceramic material. The preparation method is simple, can reduce energy consumption, shorten preparation time and reduce cost, and is suitable for mass production.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a high-strength porous silicon carbide ceramic material and a preparation method thereof.
Background
The silicon carbide-based porous ceramic is a material with both functionality and structure, has the excellent high-temperature resistance, wear resistance, acid and alkali corrosion resistance and high heat conductivity of silicon carbide, has the characteristics of high porosity, large specific surface area and light weight of a porous structure, and has important research and application values in multiple fields of filtration and separation, heat exchange and heat transfer, energy storage devices, catalyst carriers, sound absorption materials and the like.
At present, the organic foam slurry dipping method is one of the most widely applied porous silicon carbide ceramic material preparation processes, and the method comprises the steps of dipping organic foam into ceramic slurry, then burning off the organic foam and sintering into a ceramic body. However, as the organic foam is volatilized at high temperature, the pore ribs of the prepared porous silicon carbide ceramic can retain a hollow pore structure, so that the density is not high, and the main problems of reduced mechanical strength and poor thermal shock resistance exist.
Traditionally, in order to improve the strength of porous silicon carbide ceramic materials, a secondary slurry coating process for increasing the amount of organic foam adhesive slurry or a siliconizing treatment for filling holes of hole ribs by permeating other substances is adopted. Compared with the basic slurry dipping method, the secondary slurry coating process has more secondary slurry coating and secondary sintering processes, and can not eliminate holes, so that the improvement of strength is limited; the siliconizing treatment is influenced by the mesh size and the diameter of the hole rib of the porous silicon carbide ceramic and whether the blind hole is blocked, secondary high-temperature sintering is needed, the preparation process is complicated, and the content of residual silicon is high.
The preparation method has the obvious advantages that the holes of the porous silicon carbide ceramic material pore ribs can be effectively eliminated or reduced without secondary sintering in the preparation process, the content of residual silicon is extremely low, the strength and the thermal shock resistance of the porous silicon carbide ceramic material can be obviously improved, and the application of the porous silicon carbide ceramic material in engineering environments with high impact force, high stress, high temperature change and the like is increased.
Disclosure of Invention
The invention provides a high-strength porous silicon carbide ceramic material and a preparation method thereof, aiming at improving the mechanical and thermal properties of the porous silicon carbide ceramic material, prolonging the service life and simplifying the traditional preparation process for improving the strength of the porous silicon carbide ceramic material. The porous silicon carbide ceramic material prepared by the method does not need secondary sintering, can effectively eliminate or reduce holes of the pore ribs, has extremely low residual silicon content, and obviously improves the strength and thermal shock resistance of the porous silicon carbide ceramic material.
The method comprises the following specific steps:
step 1: soaking the polyurethane sponge in the required shape for 2 hours by using 10-30 wt% of sodium hydroxide solution;
step 2: preparing slurry A and slurry B, wherein the slurry A comprises the following components: x wt% of silicon powder, 1-X wt% of thermosetting resin and 2000-5000 meshes of particle size; the components of the slurry B are as follows: 45-75 wt% of silicon carbide powder, 3000-5000 meshes of particle size, 2-5 wt% of alumina and 20-53 wt% of thermosetting resin, and mechanically stirring the silicon carbide powder, the alumina and the thermosetting resin for 15 minutes at a rotation speed of 1500r/min to obtain slurry A and slurry B;
and step 3: soaking the polyurethane sponge treated in the step 1 into the slurry A, completely filling the slurry A into the polyurethane sponge, extruding the redundant slurry out, wherein the extrusion ratio is (4:1) - (6:1), and placing the polyurethane sponge in an oven at 80 ℃ for heating for 5 minutes for semi-curing;
and 4, step 4: soaking the semi-cured polyurethane sponge adhered with the slurry A in the step 3 into the slurry B to enable the slurry B to completely fill the interior of the sponge, removing redundant slurry in an air blowing or centrifugal mode, and placing the sponge in an oven at 80 ℃ for heating for 15 minutes to cure to obtain a high-strength porous silicon carbide ceramic precursor;
and 5: and (4) placing the high-strength porous silicon carbide ceramic precursor obtained in the step (4) into a high-temperature furnace, and sintering for 2 hours at 1550-1900 ℃ in a vacuum, nitrogen or inert protective atmosphere to obtain the high-strength porous silicon carbide ceramic material.
The density range of the pores of the polyurethane sponge obtained in the step 1 is 10-50 PPI, namely the pore diameter is 0.5-3 mm.
The components of the slurry A in the step 2 comprise silicon powder with the mass fraction of X and thermosetting resin with the mass fraction of 1-X, wherein X is determined by the following formula, wherein eta is the carbon residue rate of the thermosetting resin, and the proportion is adopted because the silicon powder needs to react with both the thermosetting resin carbon residue and the polyurethane carbon residue, and no residual silicon or residual carbon is generated.
The thermosetting resin in the slurry A and the slurry B in the step 2 is resin with high carbon yield, and includes but is not limited to phenolic resin, furfural resin and epoxy resin.
The extrusion ratio of the step 3 is the ratio of the thickness before extrusion to the thickness during extrusion, the larger the extrusion ratio is, the smaller the thickness of the slurry adhered to the pore ribs of the polyurethane sponge is, the larger the pore diameter is, and the higher the porosity is.
The high-strength porous silicon carbide ceramic material obtained in the step 5 has the same gap three-dimensional structure as polyurethane foam, the inner layer of the pore rib is reaction-sintered silicon carbide, the surface layer of the pore rib is powder-sintered silicon carbide, pores of the pore rib can be effectively eliminated or reduced, and the content of residual silicon is extremely low (lower than 5%).
The invention has the advantages of
The invention provides a high-strength porous silicon carbide ceramic material and a preparation method thereof, wherein the high-strength porous silicon carbide ceramic material is prepared by reacting and sintering silicon powder in a first layer of slurry with residual carbon generated by cracking of a polyurethane pore rib, so that a hollow structure of the pore rib is reduced or even eliminated, secondary slurry dipping can be carried out before sintering, and the mechanical strength and the thermal shock resistance of the porous silicon carbide ceramic material are further improved.
Respectively carbonizing the thermosetting resin and the polyurethane porous filament at 230-800 ℃ during roasting, and reacting the residual carbon of the thermosetting resin and the polyurethane porous filament with silicon in the slurry A to generate silicon carbide at 1550-1900 ℃; the crystal grains in the slurry B gradually grow along with the increase of the temperature, and a crystal boundary is formed among the grains until the grains are completely compact. Compared with the traditional secondary slurry coating process, the method can effectively eliminate or reduce holes of the porous silicon carbide ceramic material hole ribs and improve the density of the porous silicon carbide ceramic hole ribs; compared with siliconizing treatment, the method does not need secondary high-temperature sintering, and the content of residual silicon is extremely low, so that the key problem of low strength of the porous silicon carbide ceramic material is fundamentally solved.
The preparation method is simple, can reduce energy consumption, shorten preparation time and reduce cost, and is suitable for mass production.
Drawings
FIG. 1 is a flow chart showing the steps of the present invention;
FIG. 2 is a photograph showing a comparison of the structure of a porous silicon carbide ceramic rib
FIG. 3 is a graph showing the mechanical properties of a high-strength porous silicon carbide ceramic material
Detailed Description
Example 1 (phenolic resin)
Firstly, soaking a polyurethane sponge with the pore density of 10PPI in a 10 wt% sodium hydroxide solution for 2 hours for pretreatment, then soaking the treated polyurethane sponge in the prepared slurry A to enable the slurry A to completely fill the interior of the polyurethane sponge, extruding the redundant slurry with the extrusion ratio of 4:1, and placing the polyurethane sponge in an oven at 80 ℃ for heating for 5 minutes for semi-solidification. And then soaking the semi-cured polyurethane sponge adhered with the slurry A into the slurry B to enable the slurry B to completely fill the interior of the sponge, removing the redundant slurry in an air blowing mode, and heating the sponge in an oven at 80 ℃ for 15 minutes to cure the sponge. And finally, placing the ceramic material in a high-temperature furnace, and sintering the ceramic material for 2 hours at 1600 ℃ under the protection of nitrogen to obtain the high-strength porous silicon carbide ceramic material.
The slurry A comprises the following components: 60 wt% of silicon powder, 40 wt% of phenolic resin and 2000-mesh particle size; the components of the slurry B are as follows: 45% of silicon carbide powder, 3000 meshes of particle size, 5% of alumina and 50% of phenolic resin by weight.
When the particle sizes of the silicon powder and the silicon carbide powder are too small, agglomeration is easy to occur, and uniform dispersion is difficult; when the particle size is too large, sintering and molding are difficult, and the energy required by sintering and molding is large, so that sintering and densification are difficult.
As shown in fig. 2, the high-strength porous silicon carbide ceramic pore rib structure prepared in this embodiment is shown, and it can be seen from the figure that the porous rib hollow structure is eliminated and the density is increased after the silicon powder reacts and sinters with the carbon residue generated by the polyurethane pore rib. Fig. 3 is a mechanical property curve of the high-strength porous silicon carbide ceramic material prepared in this embodiment, which is improved by 1.2 times compared with the strength of the porous silicon carbide ceramic prepared by the basic slurry dipping method, and thus it can be seen that the present invention can effectively eliminate or reduce the holes of the pore ribs.
Example 2 (Furfural resin)
Firstly, soaking a polyurethane sponge with the pore density of 10PPI in a 10 wt% sodium hydroxide solution for 2 hours for pretreatment, then soaking the treated polyurethane sponge in the prepared slurry A to enable the slurry A to completely fill the interior of the polyurethane sponge, extruding the redundant slurry with the extrusion ratio of 4:1, and placing the polyurethane sponge in an oven at 80 ℃ for heating for 5 minutes for semi-solidification. And then soaking the semi-cured polyurethane sponge adhered with the slurry A into the slurry B to enable the slurry B to completely fill the interior of the sponge, removing the redundant slurry in an air blowing mode, and heating the sponge in an oven at 80 ℃ for 15 minutes to cure the sponge. And finally, placing the ceramic material in a high-temperature furnace, and sintering the ceramic material for 2 hours at 1600 ℃ under the protection of nitrogen to obtain the high-strength porous silicon carbide ceramic material.
The slurry A comprises the following components: 65 wt% of silicon powder, 35 wt% of furfural resin and 3000-mesh particle size; the components of the slurry B are as follows: 55% of silicon carbide powder, 4000 meshes of particle size, 5% of alumina and 40% of furfural resin by weight.
Claims (5)
1. A preparation method of a high-strength porous silicon carbide ceramic material is characterized by comprising the following specific steps:
step 1: soaking the polyurethane sponge in the required shape for 2 hours by using 10-30 wt% of sodium hydroxide solution;
step 2: preparing slurry A and slurry B, wherein the slurry A comprises the following components: x wt% of silicon powder, 1-X wt% of thermosetting resin and 2000-5000 meshes of particle size; the components of the slurry B are as follows: 45-75 wt% of silicon carbide powder, 3000-5000 meshes of particle size, 2-5 wt% of alumina and 20-53 wt% of thermosetting resin, and mechanically stirring the silicon carbide powder, the alumina and the thermosetting resin for 15 minutes at a rotation speed of 1500r/min to obtain slurry A and slurry B;
and step 3: soaking the polyurethane sponge treated in the step 1 into the slurry A, completely filling the slurry A into the polyurethane sponge, extruding the redundant slurry out, wherein the extrusion ratio is (4:1) - (6:1), and placing the polyurethane sponge in an oven at 80 ℃ for heating for 5 minutes for semi-curing; the extrusion ratio is the ratio of the thickness before extrusion to the thickness during extrusion;
and 4, step 4: soaking the semi-cured polyurethane sponge adhered with the slurry A in the step 3 into the slurry B to enable the slurry B to completely fill the interior of the sponge, removing redundant slurry in an air blowing or centrifugal mode, and placing the sponge in an oven at 80 ℃ for heating for 15 minutes to cure to obtain a high-strength porous silicon carbide ceramic precursor;
and 5: and (4) placing the high-strength porous silicon carbide ceramic precursor obtained in the step (4) into a high-temperature furnace, and sintering for 2 hours at 1550-1900 ℃ in a vacuum, nitrogen or inert protective atmosphere to obtain the high-strength porous silicon carbide ceramic material.
The density range of the pores of the polyurethane sponge obtained in the step 1 is 10-50 PPI, namely the pore diameter is 0.5-3 mm.
The mass fraction X of the silicon powder in the slurry A in the step 2 is determined by the following formula,
wherein eta is the carbon residue rate of the thermosetting resin.
2. The method for preparing a high-strength porous silicon carbide ceramic material according to claim 1, wherein the thermosetting resin in the slurry A and the slurry B in the step 2 is phenolic resin, furfural resin or epoxy resin.
3. The method for preparing a high-strength porous silicon carbide ceramic material according to claim 1, wherein the extrusion ratio of step 3 is larger, the thickness of the slurry adhered to the polyurethane sponge pore ribs is smaller, the pore size is larger, and the porosity is higher.
4. The method for preparing a high-strength porous silicon carbide ceramic material according to claim 1, wherein the high-strength porous silicon carbide ceramic material of step 5 has the same void three-dimensional structure as polyurethane foam, the inner layer of the cell ribs is reaction-sintered silicon carbide, and the surface layer is powder-sintered silicon carbide.
5. A high-strength porous silicon carbide ceramic material prepared by the preparation method according to any one of claims 1 to 4.
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