CN112047742B - Low-cost preparation method of large-size silicon nitride nanobelt aerogel - Google Patents
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Abstract
The invention belongs to the field of novel inorganic nano porous materials, and relates to a low-cost preparation method of large-size silicon nitride nanobelt aerogel. The large-size silicon nitride nanobelt aerogel low-cost preparation method comprises the steps of taking metal Si powder and silica sol as silicon sources, taking nitrogen as a nitrogen source, adding a dispersing agent and a foaming agent, foaming, curing gel, discharging and burning a pore-forming agent to form porous Si-SiO2A network; porous Si-SiO2The network is used as a silicon source for generating the silicon nitride nanobelt by the nitridation reaction, and simultaneously provides a space and a template for the growth of the silicon nitride, and Si-SiO is carried out along with the nitridation reaction2The network is consumed and the silicon nitride nanoribbons are grown in large numbers and interwoven and interconnected into a macroscopic three-dimensional silicon nitride nanoribbon aerogel. The invention reduces the manufacturing cost and solves the technical problem that the aerogel is difficult to prepare large-size products.
Description
Technical Field
The invention belongs to the field of novel inorganic nano porous materials, and particularly relates to a low-cost preparation method of large-size silicon nitride nanobelt aerogel.
Background
The ceramic aerogel is a nano-scale mesoporous composite material with high temperature resistance, high specific surface area, ultrahigh air holes and extremely low thermal conductivity, and has great application potential in the fields of high-temperature heat insulation systems, catalyst carriers, filters, electronics, optics and the like. However, the conventional ceramic aerogel is generally composed of nanoparticles, has low strength and high brittleness, is difficult to be manufactured into a large-sized product, and undergoes volume shrinkage at high temperature. Therefore, practical applications thereof have been limited. The silicon nitride nanobelt aerogel is a novel aerogel material, not only has the characteristics of ultralight weight, heat insulation, high specific surface area, strong adsorption and the like of the aerogel, but also has the performances of high temperature resistance, oxidation resistance, corrosion resistance, high strength, high elasticity, strong field emission and the like of the silicon nitride nanobelt, and particularly makes up for the defect of large brittleness of the traditional aerogel.
The patent No. 201811626361.1 uses polycarbosilane sol and carbon fiber as main raw materials, and utilizes the in-situ growth and self-assembly technology of silicon nitride nanobelts to prepare the ultralight silicon nitride nanobelt aerogel paper, the density of which is only 5mg/cm3The porosity is as high as 99.8%. The patent number is 201910271666.3, and the silicon nitride nanobelt aerogel prepared by the supercritical drying method is used for preparing the silicon nitride aerogel with small density, high purity and large specific surface area. The silicon nitride nanobelt aerogel is a new material, most of the existing silicon nitride nanobelts take an organic ceramic precursor which is expensive and not environment-friendly as a raw material, or adopt a special drying process, the preparation process is complex, the equipment requirement is high, the raw material is not green and environment-friendly, meanwhile, the research report about large-size products is hardly available, and the industrial application of the material is greatly limited.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a low-cost preparation method of large-size silicon nitride nanobelt aerogel.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a low-cost preparation method of large-size silicon nitride nanobelt aerogel comprises the steps of taking metal Si powder and silica sol as silicon sources, taking nitrogen as a nitrogen source, adding a dispersing agent and a foaming agent, foaming, curing gel, discharging and burning a pore-forming agent to form porous Si-SiO2A network; porous Si-SiO2The network is used as a nitridation reaction to generate silicon nitride nanoSilicon source in the zone, and also provides space and template for silicon nitride growth, and Si-SiO is carried out along with nitridation reaction2The network is consumed, a large number of silicon nitride nanobelts are generated and are interwoven and interconnected to form macroscopic three-dimensional silicon nitride nanobelt aerogel, and the method comprises the following specific steps:
1) preparing slurry:
putting the silica sol, the metal Si powder, the water, the graphite and the dispersing agent into a planetary ball mill according to a certain proportion, and ball-milling and uniformly mixing to obtain stable slurry;
2) a foaming step:
adding a foaming agent into the slurry obtained in the step 1), stirring for 20min by using a stirrer, and standing at 30-45 ℃ to obtain porous slurry;
3) and (3) curing and drying:
adding a curing initiator into the porous slurry obtained in the step 2), stirring for 20min by using a stirrer, standing at 30 ℃ for 1d, and drying at 110 ℃ to constant weight to obtain porous gel;
4) and (3) carbon removal:
oxidizing the porous gel obtained in the step 3) at 500 ℃ under the protection of air to discharge carbon to constant weight to obtain porous Si-SiO2A network;
5) a nitridation reaction step:
the porous Si-SiO obtained in the step 4)2And (3) a network, under the protection of nitrogen gas, raising the temperature to 1250-1410 ℃ at the heating rate of 10-15 ℃/min, preserving the temperature at 1250-1410 ℃ for 3-10 h, and cooling along with the furnace to obtain the silicon nitride nanobelt aerogel.
The particle size of the silica sol in the step 1) is one or more of 5 nm, 10 nm, 15 nm and 25 nm.
The concentration of the silica sol in the step 1) is 5% -30%.
The dispersant in the step 1) is one or more of polyacrylamide, CAMTMENT, FS20, tetramethylethylenediamine, HH2690 and MQ-301.
The foaming agent in the step 2) is one or a mixture of two or more of sodium dodecyl benzene sulfonate, triethanolamine dodecyl sulfate, ammonium dodecyl sulfate, triethanolamine dodecyl sulfate and a nonionic surfactant in any mass ratio.
The curing initiator in the step 3) is NH4One or more of Cl and HCl acid solution;
the mass ratio of the silica sol, the graphite, the metal silicon powder, the dispersing agent, the foaming agent and the initiator in the steps 1), 2) and 3) is 100: 10-23: 4-12: 0.1-2: 2-10: 2 to 10.
The invention relates to a low-cost preparation method of large-size silicon nitride nanobelt aerogel, which adopts the technical scheme and has the following characteristics:
1. according to the method, silica sol and metal silicon are used as silicon sources, nitrogen is used as a nitrogen source, the raw materials are low in price, no toxic or harmful gas is emitted in the preparation process, and the method is green and environment-friendly;
2. in the preparation process, firstly, silica sol, silicon and graphite are prepared into slurry, and large-size and high-porosity porous Si-SiO is obtained through foaming, gel curing and decarbonization2Template, then Si reacts with nitrogen to consume Si-SiO2A template is used for generating a large number of silicon nitride nanobelts, and the nanobelts are mutually interwoven and interconnected to obtain three-dimensional large-size silicon nitride nanobelts for aerogel; the process is simple to operate, does not need supercritical drying, has low requirement on equipment and has strong safety;
3. the silicon nitride nanobelt obtained by the method through silicon-carbon in-situ reaction has high purity, small diameter (< 100 nm) and large length (>100 mu m), the silicon nitride aerogel formed by interweaving and interconnecting the nanobelts has low density, large specific surface area, good toughness, moderate strength, excellent high-temperature stability and heat-insulating property, and wide application prospect in the industrial fields of heat insulation, catalysis, filtration and the like.
Drawings
Fig. 1 and 2 are digital photographs of the silicon nitride nanobelt aerogel prepared in example 1 of the method of the present invention.
FIG. 3 is a scanning electron micrograph of the silica nitride nanobelt aerogel prepared in example 1 of the method of the present invention (scanning electron micrograph of nanobelt aerogel magnified 200 times).
FIG. 4 is a photograph of a field emission scan of a silicon nitride nanobelt aerogel prepared in example 1 of the process of the present invention (a photograph of a field emission scan of a nanobelt aerogel magnified 50000 times).
Detailed Description
The invention is described with reference to the accompanying drawings and specific examples:
example 1: putting 100 parts of 5% silica sol, 5 parts of metal silicon powder, 20 parts of graphite, 0.04 part of tetramethylethylenediamine and 2 parts of HH2690 into a planetary ball mill, and carrying out ball milling for 2 hours at 30 r/min to obtain uniform slurry; adding 4 parts of sodium dodecyl benzene sulfonate solution into the slurry, and stirring at 800 r/min for 20 min; adding 20% of NH46 parts of Cl solution, stirring for 15min at the speed of 600 r/min, preserving heat for 1d at the temperature of 35 ℃, and drying to constant weight at the temperature of 110 ℃ to obtain porous gel; putting the porous gel into a muffle furnace, keeping the temperature at 500 ℃ to constant weight, and discharging carbon to obtain porous Si-SiO2A green body; porous Si-SiO2Placing the silicon nitride nanobelt aerogel in an atmosphere furnace, circulating nitrogen, raising the temperature to 1350 ℃ at the heating rate of 15 ℃/min, preserving the heat for 8 hours, and cooling along with the furnace to obtain the silicon nitride nanobelt aerogel. The digital photograph of the prepared silicon nitride nanobelt aerogel is shown in fig. 1 and 2, the scanning electron micrograph of the nanobelt aerogel magnified 200 times is shown in fig. 3, and the field emission scanning electron micrograph of the nanobelt aerogel magnified 50000 times is shown in fig. 4.
Example 2: putting 100 parts of 6% silica sol, 7 parts of silicon metal powder, 18 parts of graphite, 0.06 part of polyacrylamide and 1.8 parts of HH2690 into a planetary ball mill, and ball-milling for 2 hours at 30 r/min to obtain uniform slurry; adding 5 parts of sodium dodecyl benzene sulfonate solution into the slurry, and stirring at 800 r/min for 20 min; adding 20% of NH46 parts of Cl solution, stirring for 15min at the speed of 600 r/min, preserving heat for 1d at the temperature of 35 ℃, and drying to constant weight at the temperature of 110 ℃ to obtain porous gel; putting the porous gel into a muffle furnace, keeping the temperature at 500 ℃ to constant weight, and discharging carbon to obtain porous Si-SiO2A green body; porous Si-SiO2Placing the mixture into an atmosphere furnace, circulating nitrogen, raising the temperature to 1400 ℃ at the heating rate of 15 ℃/min, preserving the heat for 3 h, and cooling along with the furnace to obtain the silicon nitride nanobelt aerogel.
Example 3: 100 portions of silica sol with the concentration of 4 percent, 4 portions of metal silicon powder, 22 portions of graphite, 0.05 portion of polyacrylamide,2 parts of MQ-301, and placing the mixture into a planetary ball mill to perform ball milling for 2 hours at the speed of 30 r/min to obtain uniform slurry; adding 4 parts of foaming agent into the slurry, and stirring at 800 r/min for 20 min; adding 20% of NH46 parts of Cl solution, stirring for 15min at the speed of 600 r/min, preserving heat for 1d at the temperature of 35 ℃, and drying to constant weight at the temperature of 110 ℃ to obtain porous gel; putting the porous gel into a muffle furnace, keeping the temperature at 500 ℃ to constant weight, and discharging carbon to obtain porous Si-SiO2A green body; porous Si-SiO2Placing the silicon nitride nanobelt aerogel in an atmosphere furnace, circulating nitrogen, raising the temperature to 1350 ℃ at the heating rate of 15 ℃/min, preserving the heat for 8 hours, and cooling along with the furnace to obtain the silicon nitride nanobelt aerogel.
Example 4: putting 100 parts of 5% silica sol, 5.5 parts of metal silicon powder, 18 parts of graphite, 0.06 part of polyacrylamide and 1.8 parts of HH2690 into a planetary ball mill, and ball-milling for 2 hours at 30 r/min to obtain uniform slurry; adding 5 parts of dodecyl amine sulfate solution into the slurry, and stirring at 800 r/min for 20 min; adding 20% of NH45 parts of Cl solution, stirring for 15min at the speed of 600 r/min, keeping the temperature at 35 ℃ for 1d, and drying at 110 ℃ to constant weight to obtain porous gel; putting the porous gel into a muffle furnace, keeping the temperature at 500 ℃ to constant weight, and discharging carbon to obtain porous Si-SiO2A green body; porous Si-SiO2Placing the mixture into an atmosphere furnace, circulating nitrogen, raising the temperature to 1380 ℃ at the heating rate of 15 ℃/min, preserving the heat for 6 hours, and cooling along with the furnace to obtain the silicon nitride nanobelt aerogel.
Claims (6)
1. A low-cost preparation method of large-size silicon nitride nanobelt aerogel is characterized by comprising the following steps: the preparation method comprises the steps of taking metal Si powder and silica sol as silicon sources, taking nitrogen as a nitrogen source, adding a dispersing agent and a foaming agent, foaming, curing gel, discharging and burning a pore-forming agent to form porous Si-SiO2A network; porous Si-SiO2The network is used as a silicon source for generating the silicon nitride nanobelt by the nitridation reaction, and simultaneously provides a space and a template for the growth of the silicon nitride, and Si-SiO is carried out along with the nitridation reaction2The network is consumed, a large number of silicon nitride nanobelts are generated and are interwoven and interconnected to form macroscopic three-dimensional silicon nitride nanobelt aerogel, and the method comprises the following specific steps:
1) preparing slurry:
putting the silica sol, the metal Si powder, the water, the graphite and the dispersing agent into a planetary ball mill according to a certain proportion, and ball-milling and uniformly mixing to obtain stable slurry;
2) a foaming step:
adding a foaming agent into the slurry obtained in the step 1), stirring for 20min by using a stirrer, and standing at 30-45 ℃ to obtain porous slurry;
3) and (3) curing and drying:
adding a curing initiator into the porous slurry obtained in the step 2), stirring for 20min by using a stirrer, standing at 30 ℃ for 1d, and drying at 110 ℃ to constant weight to obtain porous gel;
4) and (3) carbon removal:
oxidizing the porous gel obtained in the step 3) at 500 ℃ under the protection of air to discharge carbon to constant weight to obtain porous Si-SiO2A network;
5) a nitridation reaction step:
the porous Si-SiO obtained in the step 4)2A network, under the protection of nitrogen, raising the temperature to 1250-1410 ℃ at a heating rate of 10-15 ℃/min, preserving the temperature at 1250-1410 ℃ for 3-10 h, and cooling along with a furnace to obtain the silicon nitride nanobelt aerogel; the mass ratio of the silica sol, the graphite, the metal silicon powder, the dispersing agent, the foaming agent and the initiator is 100: 10-23: 4-12: 0.1-2: 2-10: 2 to 10.
2. The method for preparing large-size silicon nitride nanobelt aerogel according to claim 1, wherein: the particle size of the silica sol in the step 1) is one or more of 5 nm, 10 nm, 15 nm and 25 nm.
3. The method for preparing large-size silicon nitride nanobelt aerogel according to claim 1, wherein: the concentration of the silica sol in the step 1) is 5% -30%.
4. The method for preparing large-size silicon nitride nanobelt aerogel according to claim 1, wherein: the dispersant in the step 1) is one or more of polyacrylamide, CAMTMENT, FS20, tetramethylethylenediamine, HH2690 and MQ-301.
5. The method for preparing large-size silicon nitride nanobelt aerogel according to claim 1, wherein: the foaming agent in the step 2) is one or a mixture of more than two of sodium dodecyl benzene sulfonate, dodecyl amine sulfate, lauryl triethanolamine sulfate and a nonionic surfactant in any mass ratio.
6. The method for preparing large-size silicon nitride nanobelt aerogel according to claim 1, wherein: the curing initiator in the step 3) is NH4Cl and HCl acid solution.
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