CN112811933A - Preparation method of nanowire-reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel and product thereof - Google Patents
Preparation method of nanowire-reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel and product thereof Download PDFInfo
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Abstract
The invention relates to the technical field of heat-proof materials, and particularly discloses a preparation method of a nanowire-reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel and a product thereof, wherein a ceramic slurry containing silicon powder, water, a sintering aid and albumen powder is solidified, molded and dried to prepare a blank; embedding the blank into silicon nitride powder for nitrogen sintering to obtain the nanowire reinforced silicon nitride foamed ceramic; the nanowire reinforced silicon nitride foamed ceramic is further arranged in SiO2And (3) carrying out vacuum impregnation in the sol, and then carrying out gelation, solution replacement and drying to obtain the nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel. The invention simplifies the steps of the nanowire reinforced foam ceramic, and the nanowire reinforced foam ceramicThe existence of the rice noodles enables the connection between the silicon dioxide aerogel and the ceramic to be tighter, prevents the aerogel from falling off powder and falling off, is favorable for prolonging the service life of the material, and promotes large-scale production.
Description
Technical Field
The invention relates to the technical field of heat-proof materials, in particular to a preparation method of a nanowire-reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel and a product thereof.
Background
The silicon dioxide aerogel is a porous material formed by gathering nano-scale ultrafine particles, has a continuous spatial net-shaped three-dimensional structure inside, has the characteristics of low density, high porosity, high specific surface area, low thermal conductivity and the like, and can be widely applied to the fields of high-efficiency heat insulation protection, sound insulation and noise reduction, catalyst carriers, filtration and adsorption and the like. But the aerogel also has the defects of poor inherent mechanical properties, such as low material strength and easy breakage caused by weak internal bonding force.
By using the aerogel to dip the foamed ceramic, the pore diameter of the internal channel and the pore diameter between crystal grains of the material can be reduced, the thermal conductivity of the foamed ceramic is reduced, the compression strength of the material is improved, and the dielectric property is approximately kept unchanged. The high strength, low density, good dielectric property and low thermal conductivity promote the silicon nitride foam ceramic/aerogel composite material to have great application potential in the fields of metallurgy, high-temperature filter carriers, aerospace and the like.
However, the currently disclosed patents (for example, patents CN103553693A and CN106866180A) using aerogel to impregnate foamed ceramics directly adopt aerogel sol to impregnate unmodified porous ceramics, at this time, the bonding force generated by direct contact between the ceramic pores and the aerogel is relatively weak, and the inorganic aerogel has inherent brittleness, and the structure with high porosity makes the bonding area between its primary particles small, so it is easy to break in the neck region, and powder falling and falling off occur, thereby resulting in the technical problem of poor thermal conductivity.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel and a product thereof; silicon powder is used as a raw material to prepare in-situ self-growing nanowire reinforced silicon nitride foam ceramic in one step through reaction and sintering, and then the nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material is prepared through vacuum impregnation and sol. The step of nano wire reinforcing foamed ceramics has been simplified to this process to the existence of nano wire makes to be connected more closely between silica aerogel and the pottery, prevents that the aerogel from appearing falling the powder and droing, does benefit to the life of extension material, promotes the large-scale production.
The invention provides a preparation method of a nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel, which comprises the following steps:
(1) curing, molding and drying ceramic slurry containing silicon powder, water, a sintering aid and albumen powder to obtain a blank;
(2) embedding the blank into silicon nitride powder for nitridation sintering to obtain the nanowire reinforced silicon nitride foamed ceramic;
(3) the nanowire reinforced silicon nitride foamed ceramic is further arranged in SiO2And (3) carrying out vacuum impregnation in the sol, and then carrying out gelation, solution replacement and drying to obtain the nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel.
Further, in the step (1):
the mass ratio of the silicon powder, the water, the sintering aid and the protein powder is (44-50): 41-49): 2-5): 5-10.
The sintering aid is one or more of aluminum oxide, yttrium oxide and lanthanum oxide.
The silicon powder is metal silicon powder with the purity of more than 99.9 percent, and the particle size of the silicon powder is 3-10 mu m.
Further, the step (1) specifically includes the steps of: mixing and stirring silicon powder, water and a sintering aid, adding protein powder, mixing, stirring and foaming to obtain foaming slurry, performing vibration treatment on the foaming slurry, pouring the foaming slurry into a mold, sealing and curing, demolding and drying to obtain a blank.
Further, mixing and stirring the silicon powder, the water and the sintering aid for 10-20 hours, adding the protein powder, mixing and stirring for 2-3 hours, and foaming; the curing temperature is 60-90 ℃, and the curing time is 45-60 min; the drying time is more than 72 h.
Further, in the step (2):
the purity of the silicon nitride powder is more than 99 percent.
Sintering environment: heating to 1000 ℃ at the heating rate of 10 ℃/min under the nitrogen atmosphere of 0.1MPa, heating to 1200 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 2h, heating to 1350 ℃ and 1500 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 4-12h, and cooling to room temperature along with the furnace to obtain the nanowire reinforced silicon nitride foamed ceramic.
The temperature rises to 1000 ℃ at a higher heating rate of 10 ℃/min in the initial sintering stage; si with the temperature of more than 1000 ℃ participates in the reaction, the temperature rising rate is slowed down to 5 ℃/min, and the reaction product is pre-nitrided for 2 hours at the temperature of 1200 ℃; in order to ensure the nitriding effect, the temperature is slowly raised to 1350-.
Further, SiO in the step (3)2The preparation method of the sol comprises the following steps: dissolving glacial acetic acid in water to prepare acidic water, stirring and mixing the acidic water and hexadecyl trimethyl ammonium bromide, adding methyl triethoxysilane, continuously stirring and mixing uniformly, and adjusting the pH value to 7-7.5 to obtain SiO2And (3) sol.
Furthermore, the mass ratio of the acidic water, the hexadecyl trimethyl ammonium bromide and the methyl triethoxysilane is (40-80): 1-4): 20-40, and the concentration of the glacial acetic acid in the acidic water is 0.02 mol/L.
Further, ammonia water having a concentration of 1mol/L was used to adjust the pH.
Further, in the step (3):
the vacuum degree is-80 to-100 KPa, and the vacuum impregnation time is 30 to 60 min.
The gel specifically comprises: and (3) carrying out gel aging for 8-12 h at the temperature of 60-80 ℃.
The solution replacement specifically comprises: firstly, deionized water is used for replacement for 1 time in a water bath at the temperature of 60-80 ℃, and the replacement time is 12-24 hours; and then, replacing the mixture for 3 times by absolute ethyl alcohol at normal temperature, wherein the replacement time is 12-18 h each time.
The drying specifically comprises the following steps: CO 22Supercritical drying, drying parameters: the temperature is 50-55 ℃, and the pressure is 10-12 MPa.
The invention also provides the nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel prepared by the preparation method of the nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel.
Compared with the prior art, the invention has the following beneficial effects:
the invention modifies the foamed ceramic by growing the nano-wire on the pore wall of the foamed ceramic: on one hand, the binding effect of the nanowires on aerogel in pores enables the wall of the ceramic pore to be tightly combined with the aerogel, so that the aerogel can be prevented from falling off; on the other hand, the diameter of the nanowire is close to the size of the primary particle of the aerogel, and the nanowire can be uniformly compounded with the aerogel matrix in a nanoscale to form a three-dimensional interpenetrating network, so that the aerogel is prevented from being broken. Therefore, the invention can effectively solve the technical problem of powder falling and shedding of the aerogel material and obviously prolong the service life of the material.
According to the invention, silicon powder is used as a raw material for curing and molding, and then embedded into silicon nitride powder for one-step reaction sintering to prepare the in-situ self-growing nanowire reinforced silicon nitride foamed ceramic, so that the steps of nanowire reinforced foamed ceramic are simplified, meanwhile, the prepared silicon nitride nanowire belongs to a one-dimensional nanostructure and has a very small size, and due to the size effect and the quantum effect, the prepared silicon nitride nanowire has the characteristics of high bulk phase silicon nitride atom bonding degree, strong covalent bond and good mechanical property, and has no influence on the overall thermal conductivity, density and the like of the material.
Compared with the bulk material, the silicon nitride nanowire has more complete crystals, higher surface energy and specific surface area, bending strength and elastic modulus (570GPa) of the silicon nitride nanowire are far higher than those of the bulk material, and the silicon nitride nanowire has good flexibility, and can be used for enhancing the toughness of the material and enhancing the compressive strength by utilizing the adhesive force of the material, thereby being beneficial to enhancing the toughness of the foamed ceramic/aerogel composite material.
The nano-wire in the silicon nitride foamed ceramic is modified by the in-situ self-growth of the nano-wire, so that the toughening distribution of the nano-wire is more uniform relative to the added crystal whisker, and the agglomeration problem is avoided. The silicon nitride foamed ceramic has the characteristics of high temperature resistance, corrosion resistance, thermal shock resistance, low thermal expansion coefficient and excellent thermal stability, and also has lower dielectric constant (5.6-7.8) and dielectric loss. The in-situ self-grown silicon nitride nanowire reinforced silicon nitride foam ceramic is used for promoting the toughness and the specific surface area of the material to be increased, so that the material has higher heat dissipation efficiency. Aerogel makes this combined material have low thermal conductivity, hydrophobic dampproofing characteristics, and the nano wire in the foamed ceramic hole can closely combine with compound aerogel, prevents that the breakage of aerogel from droing, does benefit to extension material life. The nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material expands the application of the nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material in the field of heat prevention and insulation.
Drawings
FIG. 1 is a microscopic morphology of nanowires in pores of the in-situ self-grown nanowire-reinforced silicon nitride foam ceramic sample prepared in example 1 under a scanning electron microscope.
FIG. 2 is a high-power microscopic morphology of nanowires in pores of the in-situ self-grown nanowire-reinforced silicon nitride foam ceramic sample prepared in example 1 under a scanning electron microscope.
FIG. 3 is a microscopic morphology of aerogel filled in pores of the foam ceramic under a scanning electron microscope of a nanowire-reinforced silicon nitride foam ceramic composite silica aerogel sample prepared in example 1.
FIG. 4 is a high-power microscopic morphology diagram of aerogel under a scanning electron microscope of a nanowire-reinforced silicon nitride foam ceramic composite silica aerogel sample prepared in example 1.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The silicon powder used in the following examples of the invention is metal silicon powder with a purity of more than 99.9%, and the particle size is 3-10 μm; the purity of the silicon nitride powder is more than 99 percent.
Example 1
Weighing 44% by mass of silicon powder, 47% by mass of deionized water, 1% by mass of alumina and 2% by mass of yttrium oxide, putting the raw materials into a ball mill, stirring for 20 hours, then adding 6% by mass of protein powder, stirring for 2 hours, and discharging to obtain slurry. And during molding, pouring the mixed slurry into a molding die. And sealing the mould by using a preservative film, putting the mould into a water bath furnace, curing for 1 hour at the temperature of 80 ℃, demoulding, and drying for more than 72 hours in the air to obtain a molded blank. And placing the blank body in a crucible, embedding silicon nitride powder around the blank body, placing the blank body in a nitriding furnace, vacuumizing the nitriding furnace, and introducing 0.1MPa nitrogen for sintering. The sintering system is as follows: the heating rate is 10 ℃/min within the range of room temperature (25 ℃) to 1000 ℃; the temperature rise rate is 5 ℃/min at 1000-1200 ℃; the heating rate of 1200 ℃ to 1350 ℃ is 1 ℃/min, the temperature of 1200 ℃ is kept for 2h, the temperature of 1350 ℃ is kept for 10h, and finally the temperature is cooled to the room temperature along with the furnace. The sintered in-situ self-grown nanowire reinforced silicon nitride foam ceramic is used as a matrix for vacuum impregnation of aerogel for later use.
Mixing and stirring 60mL of acidic deionized water (the concentration of glacial acetic acid in the acidic deionized water is 0.02mol/L) and 2g of CTAB for 20 min; adding 30mL of MTES and continuing stirring for 3 h; and then, adjusting the sol to pH 7 by using an ammonia water solution with the concentration of 1mol/L, and finishing the sol preparation. Placing the sintered silicon nitride foamed ceramic in a vacuum device for vacuum impregnation of SiO2Sol, wherein the vacuum degree is about-84 KPa, and the vacuum retention time is 30 min; after gel aging is carried out for 8 hours in a water bath at 60 ℃, deionized water is used for replacing for 1 time in the water bath at 60 ℃, and the replacement time is 12 hours; then, replacing the mixture for 3 times by absolute ethyl alcohol at normal temperature, wherein the replacement time is 12 hours each time; by using CO2And (3) obtaining the in-situ self-growing nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel material by a supercritical drying technology (the temperature is 50-55 ℃ and the pressure is 10-12 MPa).
Fig. 1 and 2 are microscopic morphologies of nanowires in pores of the in-situ self-grown silicon nitride foam ceramic sample under a high-low scanning electron microscope, respectively, and it can be found that the dense nanowires are self-grown in situ in the pore structure of the foam ceramic. Fig. 3 and 4 are microscopic morphology diagrams of aerogel impregnated in pores of the foam ceramic under a high-power scanning electron microscope respectively for in-situ self-grown nanowire-reinforced silicon nitride foam ceramic composite silica aerogel samples, and it can be found that the pores of the foam ceramic are completely filled with the silica aerogel. The room temperature thermal conductivity of the in-situ self-grown nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material prepared by the embodiment is 0.109W/(m.K).
Example 2:
weighing 44% by mass of silicon powder, 47% by mass of deionized water, 1% by mass of alumina and 2% by mass of yttrium oxide, putting the raw materials into a ball mill, stirring for 20 hours, then adding 6% by mass of protein powder, stirring for 2 hours, and discharging to obtain slurry. And during molding, pouring the mixed slurry into a molding die. And sealing the mould by using a preservative film, putting the mould into a water bath furnace, curing for 1 hour at the temperature of 80 ℃, demoulding, and drying for more than 72 hours in the air to obtain a molded blank. And placing the blank body in a crucible, embedding silicon nitride powder around the blank body, placing the blank body in a nitriding furnace, vacuumizing the nitriding furnace, and introducing 0.1MPa nitrogen for sintering. The sintering system is as follows: the heating rate is 10 ℃/min within the range of room temperature (25 ℃) to 1000 ℃; the temperature rise rate is 5 ℃/min at 1000-1200 ℃; the heating rate of 1200-1400 ℃ is 1 ℃/min, the heat preservation is carried out for 2h at 1200 ℃, the heat preservation is carried out for 8h at 1400 ℃, and finally the temperature is cooled to the room temperature along with the furnace. The sintered in-situ self-grown nanowire reinforced silicon nitride foam ceramic is used as a matrix for vacuum impregnation of aerogel for later use.
Mixing and stirring 60mL of acidic deionized water (the concentration of glacial acetic acid in the acidic deionized water is 0.02mol/L) and 2g of CTAB for 20 min; adding 30mL of MTES and continuing stirring for 3 h; and then, adjusting the sol to pH 7 by using an ammonia water solution with the concentration of 1mol/L, and finishing the sol preparation. Placing the sintered silicon nitride foamed ceramic in a vacuum device for vacuum impregnation of SiO2Sol, wherein the vacuum degree is about-84 KPa, and the vacuum retention time is 30 min; after gel aging is carried out for 8 hours in a water bath at 60 ℃, deionized water is used for replacing for 1 time in the water bath at 60 ℃, and the replacement time is 12 hours; then, replacing the mixture for 3 times by absolute ethyl alcohol at normal temperature, wherein the replacement time is 12 hours each time; by using CO2And (3) obtaining the in-situ self-growing nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel material by a supercritical drying technology (the temperature is 50-55 ℃ and the pressure is 10-12 MPa).
The room temperature thermal conductivity of the in-situ self-grown nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material prepared by the embodiment is 0.117W/(m.K).
Example 3:
weighing 44% by mass of silicon powder, 47% by mass of deionized water, 1% by mass of alumina and 2% by mass of yttrium oxide, putting the raw materials into a ball mill, stirring for 20 hours, then adding 6% by mass of protein powder, stirring for 2 hours, and discharging to obtain slurry. And during molding, pouring the mixed slurry into a molding die. And sealing the mould by using a preservative film, putting the mould into a water bath furnace, curing for 1 hour at the temperature of 80 ℃, demoulding, and drying for more than 72 hours in the air to obtain a molded blank. And placing the blank body in a crucible, embedding silicon nitride powder around the blank body, placing the blank body in a nitriding furnace, vacuumizing the nitriding furnace, and introducing 0.1MPa nitrogen for sintering. The sintering system is as follows: the heating rate is 10 ℃/min within the range of room temperature (25 ℃) to 1000 ℃; the temperature rise rate is 5 ℃/min at 1000-1200 ℃; the heating rate of 1200-1450 ℃ is 1 ℃/min, the temperature of 1200 ℃ is kept for 2h, the temperature of 1450 ℃ is kept for 8h, and finally the furnace is cooled to the room temperature. The sintered in-situ self-grown nanowire reinforced silicon nitride foam ceramic is used as a matrix for vacuum impregnation of aerogel for later use.
Mixing and stirring 60mL of acidic deionized water (the concentration of glacial acetic acid in the acidic deionized water is 0.02mol/L) and 2g of CTAB for 20 min; adding 30mL of MTES and continuing stirring for 3 h; and then, adjusting the sol to pH 7 by using an ammonia water solution with the concentration of 1mol/L, and finishing the sol preparation. Placing the sintered silicon nitride foamed ceramic in a vacuum device for vacuum impregnation of SiO2Sol, wherein the vacuum degree is about-84 KPa, and the vacuum retention time is 30 min; after gel aging is carried out for 8 hours in a water bath at 60 ℃, deionized water is used for replacing for 1 time in the water bath at 60 ℃, and the replacement time is 12 hours; then, replacing the mixture for 3 times by absolute ethyl alcohol at normal temperature, wherein the replacement time is 12 hours each time; by using CO2And (3) obtaining the in-situ self-growing nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel material by a supercritical drying technology (the temperature is 50-55 ℃ and the pressure is 10-12 MPa).
The room temperature thermal conductivity of the in-situ self-grown nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material prepared by the embodiment is 0.114W/(m.K).
Example 4:
weighing 44% by mass of silicon powder, 47% by mass of deionized water, 1% by mass of alumina and 2% by mass of yttrium oxide, putting the raw materials into a ball mill, stirring for 20 hours, then adding 6% by mass of protein powder, stirring for 2 hours, and discharging to obtain slurry. And during molding, pouring the mixed slurry into a molding die. And sealing the mould by using a preservative film, putting the mould into a water bath furnace, curing for 1 hour at the temperature of 80 ℃, demoulding, and drying for more than 72 hours in the air to obtain a molded blank. And placing the blank body in a crucible, embedding silicon nitride powder around the blank body, placing the blank body in a nitriding furnace, vacuumizing the nitriding furnace, and introducing 0.1MPa nitrogen for sintering. The sintering system is as follows: the heating rate is 10 ℃/min within the range of room temperature (25 ℃) to 1000 ℃; the temperature rise rate is 5 ℃/min at 1000-1200 ℃; the heating rate of 1200-1450 ℃ is 1 ℃/min, the temperature is kept for 2h at 1200 ℃, the temperature is kept for 12h at 1450 ℃, and finally the furnace is cooled to the room temperature. The sintered in-situ self-grown nanowire reinforced silicon nitride foam ceramic is used as a matrix for vacuum impregnation of aerogel for later use.
Mixing and stirring 60mL of acidic deionized water (the concentration of glacial acetic acid in the acidic deionized water is 0.02mol/L) and 2g of CTAB for 20 min; adding 30mL of MTES and continuing stirring for 3 h; and then, adjusting the sol to pH 7 by using an ammonia water solution with the concentration of 1mol/L, and finishing the sol preparation. Placing the sintered silicon nitride foamed ceramic in a vacuum device for vacuum impregnation of SiO2Sol, wherein the vacuum degree is about-84 KPa, and the vacuum retention time is 30 min; after gel aging is carried out for 8 hours in a water bath at 60 ℃, deionized water is used for replacing for 1 time in the water bath at 60 ℃, and the replacement time is 12 hours; then, replacing the mixture for 3 times by absolute ethyl alcohol at normal temperature, wherein the replacement time is 12 hours each time; by using CO2And (3) obtaining the in-situ self-growing nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel material by a supercritical drying technology (the temperature is 50-55 ℃ and the pressure is 10-12 MPa).
The room temperature thermal conductivity of the in-situ self-grown nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material prepared by the embodiment is 0.122W/(m.K).
Comparative example 1
The difference from example 4 is that the green compact was sintered directly in a nitriding furnace without being embedded with silicon nitride powder.
The room temperature thermal conductivity of the in-situ self-grown nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material prepared by the embodiment is 0.126W/(m.K).
Comparative example 2
The difference from example 4 is that the preparation steps of embedding the formed green body into silicon nitride powder and sintering the formed green body in nitrogen to obtain the nanowire-reinforced silicon nitride foam ceramic are omitted, and the SiO is directly performed on the existing silicon nitride foam ceramic2And (4) carrying out vacuum impregnation on the sol.
The room temperature thermal conductivity of the in-situ self-grown nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material prepared by the embodiment is 0.139W/(m.K).
Comparative example 3
The difference from example 4 is that the sintering environment of the shaped green body: directly heating from room temperature (25 ℃) to 1450 ℃ at the heating rate of 10 ℃/min, preserving heat for 12h, and finally cooling to room temperature along with the furnace.
The room temperature thermal conductivity of the in-situ self-grown nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material prepared by the embodiment is 0.133W/(m.K).
Comparative example 4
The difference from example 4 is that the sintering environment of the shaped green body: directly heating to 1200 ℃ from room temperature (25 ℃) at the heating rate of 10 ℃/min, preserving heat for 2h, then heating to 1450 ℃ at the heating rate of 5 ℃/min, preserving heat for 12h, and finally cooling to room temperature along with the furnace.
The room temperature thermal conductivity of the in-situ self-grown nanowire reinforced silicon nitride foam ceramic composite silicon dioxide aerogel material prepared by the embodiment is 0.141W/(m.K).
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel is characterized by comprising the following steps:
(1) curing, molding and drying ceramic slurry containing silicon powder, water, a sintering aid and albumen powder to obtain a blank;
(2) embedding the blank into silicon nitride powder for nitridation sintering to obtain the nanowire reinforced silicon nitride foamed ceramic;
(3) the nanowire reinforced silicon nitride foamed ceramic is further placed in vacuum for soaking SiO2And carrying out sol, gel, solution replacement and drying to obtain the nanowire reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel.
2. The method for preparing the nanowire-reinforced silicon nitride foamed ceramic composite silica aerogel according to claim 1, wherein in the step (1):
the mass ratio of the silicon powder, the water, the sintering aid and the protein powder is (44-50): 41-49): 2-5): 5-10;
the sintering aid is one or more of aluminum oxide, yttrium oxide and lanthanum oxide;
the silicon powder has a purity of more than 99.9% and a particle size of 3-10 μm.
3. The method for preparing the nanowire-reinforced silicon nitride foamed ceramic composite silica aerogel according to claim 1, wherein the step (1) specifically comprises the following steps: mixing and stirring silicon powder, water and a sintering aid, adding protein powder, mixing, stirring and foaming to obtain foaming slurry, performing vibration treatment on the foaming slurry, pouring the foaming slurry into a mold, sealing and curing, demolding and drying to obtain a blank.
4. The preparation method of the nanowire reinforced silicon nitride foamed ceramic composite silica aerogel according to claim 3, wherein the silicon powder, the water and the sintering aid are mixed and stirred for 10-20 hours, and then the protein powder is added to be mixed, stirred and foamed for 2-3 hours; the curing temperature is 60-90 ℃, and the curing time is 45-60 min; the drying time is more than 72 h.
5. The method for preparing the nanowire-reinforced silicon nitride foamed ceramic composite silica aerogel according to claim 1, wherein in the step (2):
the purity of the silicon nitride powder is more than 99 percent;
sintering environment: heating to 1000 ℃ at the heating rate of 10 ℃/min under the nitrogen atmosphere of 0.1MPa, heating to 1200 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 2h, heating to 1350 ℃ and 1500 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 4-12h, and cooling to room temperature along with the furnace to obtain the nanowire reinforced silicon nitride foamed ceramic.
6. The method for preparing the nanowire-reinforced silicon nitride foamed ceramic composite silica aerogel according to claim 1, wherein SiO in the step (3)2The preparation method of the sol comprises the following steps: dissolving glacial acetic acid in water to prepare acidic water, stirring and mixing the acidic water and hexadecyl trimethyl ammonium bromide, adding methyl triethoxysilane, continuously stirring and mixing uniformly, and adjusting the pH value to 7-7.5 to obtain SiO2And (3) sol.
7. The method for preparing the nanowire reinforced silicon nitride foamed ceramic composite silica aerogel according to claim 6, wherein the mass ratio of the acidic water, the hexadecyl trimethyl ammonium bromide and the methyl triethoxysilane is (40-80): 1-4): 20-40, and the concentration of the glacial acetic acid in the acidic water is 0.02 mol/L.
8. The method for preparing the nanowire-reinforced silicon nitride foamed ceramic composite silica aerogel according to claim 6, wherein ammonia water with a concentration of 1mol/L is used for adjusting the pH value.
9. The method for preparing the nanowire-reinforced silicon nitride foamed ceramic composite silica aerogel according to claim 1, wherein in the step (3):
the vacuum degree is-80 to-100 KPa, and the vacuum impregnation time is 30 to 60 min;
the gel specifically comprises: aging the gel at 60-80 ℃ for 8-12 h;
the solution replacement specifically comprises: replacing the deionized water for 1 time in a water bath at the temperature of 60-80 ℃, wherein the replacement time is 12-24 h; then, replacing for 3 times by absolute ethyl alcohol at normal temperature, wherein the replacement time is 12-18 h each time;
the drying specifically comprises the following steps: CO 22Supercritical drying, drying parameters: the temperature is 50-55 ℃, and the pressure is 10-12 MPa.
10. A nanowire-reinforced silicon nitride foamed ceramic composite silica aerogel prepared according to the method for preparing a nanowire-reinforced silicon nitride foamed ceramic composite silica aerogel according to any one of claims 1 to 9.
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