CN115521162B - Preparation method of hollow silicon carbide microbeads - Google Patents
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Abstract
The application discloses a preparation method of hollow silicon carbide microbeads, which comprises the steps of mixing lamellar graphene with silica sol, adding an ethanol aqueous solution, sequentially carrying out ageing, modification and solvent replacement treatment, carrying out grading drying treatment, obtaining aerogel, crushing aerogel, carrying out spherical shaping machine treatment, obtaining aerogel microbeads, carrying out coating treatment on the aerogel microbeads, carrying out drying, curing and carbonization treatment, obtaining porous graphite microbeads, adding silicon powder, carrying out sintering treatment, and obtaining hollow carbonized microbeads.
Description
Technical Field
The application relates to the technical field of inorganic filler preparation, in particular to a preparation method of hollow silicon carbide microbeads.
Background
The hollow silicon carbide microbeads have the advantages of light weight, high wear resistance, high strength and the like, can be compounded with materials such as magnesium alloy, aluminum alloy, titanium alloy, stainless steel and the like to prepare a metal composite material with light weight, high strength, low expansion ratio and the like, can be compounded with the magnesium alloy to prepare a composite light material with high strength and excellent flame retardance, can be applied to warships, can be compounded with the stainless steel to prepare bulletproof armor, can greatly lighten the quality of the bulletproof armor and improve the strength of the bulletproof armor while maintaining the bulletproof armor strength, can be compounded with the aluminum alloy to prepare an ultra-light aluminum alloy applied to an airplane, and has the advantages of high temperature resistance, light weight, small expansion coefficient, high thermal conductivity and the like.
The patent CN111825094A adopts the expandable graphite powder with superfine high expansion coefficient as a raw material, sucrose or phenolic resin and silica powder are mixed to prepare slurry, the expandable graphite powder is coated with the slurry, and the hollow silicon carbide microbeads can be prepared after curing, drying, sintering and grinding treatment, but in the preparation process, the silicon source and the carbon source are difficult to fully contact, and meanwhile, the expandable graphite powder is difficult to uniformly disperse in a preparation raw material system, so that the prepared hollow silicon carbide microbeads have lower strength.
The patent CN112047343A adopts graphene oxide and carbon nano tubes to prepare aerogel microbeads, then adopts sucrose solution or phenolic resin to carry out coating treatment on the aerogel microbeads, prepares porous graphite microbeads through curing and carbonization processes, adds silica sol to prepare hollow silicon carbide microbeads after heating curing and sintering treatment, but in the preparation process, a silicon source and a carbon source are difficult to fully contact, and the prepared hollow silicon carbide microbeads have lower strength and higher carbon content.
Disclosure of Invention
In order to solve the problems that a silicon source and a carbon source are difficult to fully contact in the prior art, the prepared hollow silicon carbide microbeads are low in strength and difficult to control in morphology, and the hollow silicon carbide microbeads are difficult to form a compact structure, the first aspect of the application discloses a preparation method of the hollow silicon carbide microbeads, which comprises the following steps:
step one: mixing the layered graphene with silica sol, adding an ethanol aqueous solution, mixing to obtain mixed sol, and adding ammonia water to form alcohol gel; then adding an ageing agent, a modifying agent and a displacing medium to perform ageing treatment, modifying treatment and solvent displacing treatment respectively, and then placing the alcohol gel subjected to solvent displacing treatment in an air flow dryer to perform grading drying treatment to prepare aerogel;
step two: crushing the aerogel into fine-grain aerogel by adopting an airflow crusher, and then treating the fine-grain aerogel by adopting a spherical shaper to prepare aerogel microbeads;
coating the aerogel microbeads with a coating agent, preparing porous graphite microbeads after drying, curing and carbonizing, mixing silicon powder with the porous graphite microbeads, and sintering in a silicon carbide sintering furnace to obtain hollow silicon carbide microbeads;
in some embodiments of the application, the aging agent is a combination of silica sol and 95% ethanol aqueous solution, the aging treatment temperature is 40-60 ℃, and the aging treatment time is 10-20 hours;
in some embodiments of the application, the modifier is one of trimethylchlorosilane and hexamethyldisilazane, the modification treatment temperature is 40-60 ℃, and the modification treatment time is 100-140min;
in some embodiments of the application, the displacing medium is n-hexane;
in some embodiments of the application, the solvent displacement treatment comprises the specific steps of:
adding n-hexane into the modified alcohol gel for solvent replacement treatment, wherein the solvent replacement treatment temperature is 40-50 ℃, and the solvent replacement treatment time is 3-5h;
in one embodiment of the present application, the layer-shaped graphene in the first step includes a few-layer graphene and a multi-layer graphene, the number of layers of the few-layer graphene is 3-10, and the number of layers of the multi-layer graphene is 11-30;
in one embodiment of the present application, the coating agent in the second step includes one of a phenolic resin and a sucrose solution;
in one embodiment of the application, the layered graphene accounts for 2-4% by mass, the silica sol accounts for 10-15% by mass, the ethanol aqueous solution accounts for 5-8% by mass, the ammonia water accounts for 0.06-0.12% by mass, the aging agent accounts for 10-15% by mass, the modifier accounts for 10-15% by mass, the displacing medium accounts for 10-15% by mass, the coating agent accounts for 10-15% by mass, and the silicon powder accounts for 20-30% by mass;
in one embodiment of the present application, the gel is put into an air dryer for staged drying treatment in the first step, the primary drying treatment temperature is 60-80 ℃, the primary drying treatment time is 1-3 hours, the secondary drying treatment temperature is 80-120 ℃, the secondary drying treatment time is 1-3 hours, the tertiary drying treatment temperature is 120-150 ℃, and the tertiary drying treatment time is 1-3 hours;
in one embodiment of the present application, the specific steps of the drying treatment in the second step are:
drying by using an air flow dryer, wherein the inlet temperature of the air flow dryer is 240-260 ℃, the outlet temperature of the air flow dryer is 60-80 ℃, and the drying time is 10-40s;
in one embodiment of the present application, the curing time in the second step is 2-4 hours, and the curing temperature is 120-160 ℃;
in one embodiment of the application, the carbonization time in the second step is 1-4h, and the carbonization temperature is 400-800 ℃;
in one embodiment of the present application, the sintering treatment time in the step two is 2-6 hours in a silicon carbide sintering furnace, and the sintering treatment temperature is 1400-2000 ℃.
Compared with the prior art, the application has the following technical effects:
(1) The hollow silicon carbide microbead shell prepared by the method is composed of compact silicon carbide, so that the compressive strength and the tensile strength of the hollow silicon carbide microbead are effectively enhanced, a netlike silicon carbide skeleton is formed inside the hollow silicon carbide microbead and is filled with ultra-light aerogel, the weight of the hollow silicon carbide microbead is greatly reduced, the strength of the hollow silicon carbide microbead is effectively enhanced, the problem of breakage of the hollow silicon carbide microbead is avoided, the hollow light, high-strength and low-expansion-ratio metal composite material can be prepared by compounding the hollow light, high-strength and low-expansion-ratio metal composite material, and the problem of breakage and breakage of the composite material is effectively avoided when the metal composite material is subjected to thread processing.
(2) The layered graphene is fully contacted with the silica sol, the layered graphene is uniformly distributed in the silica sol, a silicon source and a carbon source can be fully reacted, the compressive strength and the tensile strength of the hollow silicon carbide microbeads can be effectively enhanced, meanwhile, the layered graphene is distributed in a layered or honeycomb shape in the silica sol to form a compact silicon carbide skeleton with better strength, the compressive strength of the hollow silicon carbide microbeads is enhanced, and the density of the hollow silicon carbide microbeads is improved.
Detailed Description
In order that the above-recited objects, features and advantages of the present application will become more apparent, a more particular description of the application will be rendered by reference to specific embodiments thereof.
Example 1
Step one: 3-10 layers of few-layer graphene (purchased from Anhui Mu Jia new material technology Co., ltd.) with the mass percent of 2% are mixed with silica sol (the silica content of the silica sol is 30% and the silica sol is purchased from Zhengzhou cloud trauma chemical industry Co., ltd.), 95% ethanol aqueous solution with the mass percent of 7% is added, mixed sol is obtained, and then ammonia water with the mass percent of 0.06% is added to form alcohol gel;
then adding an aging agent consisting of 3 mass percent of silica sol and 9 mass percent of 95 percent ethanol water solution to age the alcohol gel, wherein the aging temperature is 40 ℃ and the aging time is 10 hours; then adding 12.94% by mass of trimethylchlorosilane for modification treatment, wherein the modification treatment temperature is 40 ℃, the modification treatment time is 100min, then adding 13% by mass of n-hexane for solvent replacement treatment again, the replacement treatment temperature is 40 ℃, and the solvent replacement treatment time is 3h;
then placing the alcohol gel subjected to solvent replacement treatment in a dryer for grading drying treatment, wherein the primary drying treatment temperature is 60 ℃, the primary drying treatment time is 1h, the secondary drying treatment temperature is 80 ℃, the secondary drying treatment time is 1h, the tertiary drying treatment temperature is 120 ℃, and the tertiary drying treatment time is 1h, so as to prepare aerogel;
step two: crushing the aerogel into fine aerogel particles by adopting an airflow crusher, wherein the particle size is as follows: treating the fine aerogel particles with a spherical shaper at a rotation speed of 2000rpm for 80min to obtain aerogel microbeads, wherein the rotation speed of a cylindrical grinding block medium in the spherical shaper is 75-100 um;
adding a 13% sucrose solution (18 g sucrose is dissolved in distilled water and the volume is fixed to 100 ml) to perform coating treatment on aerogel microbeads, drying by adopting an air flow dryer, wherein the inlet temperature of the air flow dryer is 240 ℃, the outlet temperature of the air flow dryer is 60 ℃, the drying treatment time is 10s, then curing treatment is performed in the dryer for 2h, the curing treatment temperature is 120 ℃, carbonization treatment is performed in a muffle furnace for 1h, the carbonization treatment temperature is 400 ℃, porous graphite microbeads are prepared, silicon powder (purchased from Shandong De crystal fire Co.) with the particle size of 3000 meshes and the porous graphite microbeads are mixed, sintering treatment is performed in a silicon carbide sintering furnace, the sintering treatment time is 2h, and the sintering treatment temperature is 1400 ℃ to prepare hollow silicon carbide microbeads.
The particle size, isostatic strength and density of the hollow silicon carbide microbeads prepared according to JC/T2284-2014 standard test are as follows:
the hollow silicon carbide microbeads have the grain size of 75-100um, the isostatic pressure (hydrostatic pressure) strength of 135Mpa and the density of 0.458g/cm 3 。
Example two
Step one: 3-10 layers of few-layer graphene (purchased from Anhui Mu Jia new material technology Co., ltd.) with the mass percent of 3% are mixed with 15% of silica sol (the silica content in the silica sol is 30% and the silica sol is purchased from Zhengzhou cloud trauma chemical industry Co., ltd.), and a 95% ethanol aqueous solution with the mass percent of 7% is added, the mixed sol is obtained after mixing, and then ammonia water with the mass percent of 0.09% is added to form alcohol gel;
then adding an aging agent consisting of 3 mass percent of silica sol and 10 mass percent of 95 percent ethanol water solution to age the alcohol gel, wherein the aging temperature is 50 ℃, and the aging time is 14 hours; adding 14.91% by mass of trimethylchlorosilane for modification treatment at 50 ℃ for 120min, adding 15% by mass of n-hexane for solvent replacement treatment again at 45 ℃ for 4h;
then placing the alcohol gel subjected to solvent replacement treatment in a dryer for grading drying treatment, wherein the primary drying treatment temperature is 70 ℃, the primary drying treatment time is 2 hours, the secondary drying treatment temperature is 100 ℃, the secondary drying treatment time is 2 hours, the tertiary drying treatment temperature is 130 ℃, and the tertiary drying treatment time is 2 hours, so as to prepare aerogel;
step two: crushing the aerogel into fine aerogel particles by adopting an airflow crusher, wherein the particle size is as follows: treating the fine aerogel particles with a spherical shaper at a speed of 2500rpm for 120min to obtain aerogel microbeads, wherein the speed of rotation of a cylindrical grinding block medium in the spherical shaper is 75-100 um;
adding a 10% sucrose solution (22 g sucrose is dissolved in distilled water and the volume is fixed to 100 ml) with the weight percentage of 22% to carry out coating treatment on aerogel microbeads, adopting an air flow dryer to carry out drying treatment, wherein the inlet temperature of the air flow dryer is 250 ℃, the outlet temperature of the air flow dryer is 70 ℃, the drying treatment time is 30s, then carrying out curing treatment in the dryer, the curing treatment time is 3h, the curing treatment temperature is 140 ℃, carrying out carbonization treatment in a muffle furnace, the carbonization treatment time is 3h, the carbonization treatment temperature is 500 ℃, preparing porous graphite microbeads, mixing silicon powder with the particle size of 3000 meshes and the weight percentage of 22% (purchased from Shandong Texas crystal fire company), carrying out sintering treatment in a silicon carbide sintering furnace, the sintering treatment time is 4h, and the sintering treatment temperature is 1800 ℃ to prepare hollow silicon carbide microbeads.
The particle size, isostatic strength and density of the hollow silicon carbide microbeads prepared according to JC/T2284-2014 standard test are as follows:
the hollow silicon carbide microbeads have the particle size of 75-100um, the isostatic pressure (hydrostatic pressure) strength of 140Mpa and the density of 0.5g/cm 3 。
Example III
Step one: mixing 11-30 layers of multilayer graphene (purchased from Anhui Mu Jia new material technology Co., ltd.) with 14% of silica sol (30% of silica content in silica sol, purchased from Zhengzhou cloud wound chemical product Co., ltd.) in percentage by mass, adding 6% of 95% ethanol aqueous solution, mixing to obtain mixed sol, and adding 0.12% of ammonia water to form alcohol gel;
then adding an aging agent consisting of 4% of silica sol and 10% of 95% of ethanol water solution to age the alcohol gel, wherein the aging temperature is 60 ℃ and the aging time is 20 hours; then adding 13.88 mass percent of hexamethyldisilazane for modification treatment, wherein the modification treatment temperature is 60 ℃, the modification treatment time is 140min, then adding 14 mass percent of n-hexane for solvent replacement treatment again, the replacement treatment temperature is 50 ℃, and the solvent replacement treatment time is 5h;
then placing the alcohol gel subjected to solvent replacement treatment in a dryer for grading drying treatment, wherein the primary drying treatment temperature is 80 ℃, the primary drying treatment time is 3 hours, the secondary drying treatment temperature is 120 ℃, the secondary drying treatment time is 3 hours, the tertiary drying treatment temperature is 150 ℃, and the tertiary drying treatment time is 3 hours, so as to prepare aerogel;
step two: crushing the aerogel into fine aerogel particles by adopting an airflow crusher, wherein the particle size is as follows: treating the fine aerogel particles with a spherical shaper at a speed of 3000rpm for 150min to obtain aerogel microbeads;
adding 11 mass percent of phenolic resin (purchased from Shanghai Michelin Biochemical technologies Co., ltd., purity: BR) to carry out coating treatment on aerogel microbeads, adopting an air flow dryer to carry out drying treatment, wherein the inlet temperature of the air flow dryer is 260 ℃, the outlet temperature of the air flow dryer is 80 ℃, the drying treatment time is 40s, then carrying out curing treatment in the dryer, the curing treatment time is 4 hours, the curing treatment temperature is 160 ℃, carrying out carbonization treatment in a muffle furnace, the carbonization treatment time is 4 hours, the carbonization treatment temperature is 800 ℃, preparing porous graphite microbeads, mixing silicon powder (purchased from Shandong Texas Crystal fire Co., ltd.) with the particle size of 3000 meshes in mass percent with the porous graphite microbeads, and carrying out sintering treatment in a silicon carbide sintering furnace, wherein the sintering treatment time is 6 hours, and the sintering treatment temperature is 2000 ℃, thus obtaining the hollow silicon carbide microbeads.
The particle size, isostatic strength and density of the hollow silicon carbide microbeads prepared according to JC/T2284-2014 standard test are as follows:
the hollow silicon carbide microbeads have the particle size of 75-100um, the isostatic pressure (hydrostatic pressure) strength of 138Mpa and the density of 0.6g/cm 3 。
According to the application, the layered graphene and the silica sol are directly mixed to prepare aerogel, the aerogel is crushed and treated by a spherical shaper to prepare aerogel microbeads, the aerogel is subjected to coating treatment, then dried, solidified and carbonized to obtain porous graphite microbeads, and then silicon powder is added to prepare hollow silicon carbide microbeads after sintering treatment.
The application has been described in detail in connection with the specific embodiments and exemplary examples thereof, but such description is not to be construed as limiting the application. It will be understood by those skilled in the art that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present application and its embodiments without departing from the spirit and scope of the present application, and these fall within the scope of the present application. The scope of the application is defined by the appended claims.
Claims (1)
1. The preparation method of the hollow silicon carbide microbeads is characterized by comprising the following steps of:
step one: mixing the layered graphene with silica sol, adding an ethanol aqueous solution, mixing to obtain mixed sol, and adding ammonia water to form alcohol gel; then adding an ageing agent, a modifying agent and a displacing medium to perform ageing treatment, modifying treatment and solvent displacing treatment respectively, and then placing the alcohol gel subjected to solvent displacing treatment in an air flow dryer to perform grading drying treatment, wherein the primary drying treatment temperature is 60-80 ℃, the primary drying treatment time is 1-3h, the secondary drying treatment temperature is 80-120 ℃, the secondary drying treatment time is 1-3h, the tertiary drying treatment temperature is 120-150 ℃, and the tertiary drying treatment time is 1-3h, so as to prepare aerogel;
the layered graphene comprises fewer layers of graphene and multiple layers of graphene, wherein the number of layers of the fewer layers of graphene is 3-10, and the number of layers of the multiple layers of graphene is 11-30;
the aging agent is a mixture of silica sol and 95% ethanol water solution, the aging treatment temperature is 40-60 ℃, and the aging treatment time is 10-20 hours; the modifier is one of trimethylchlorosilane and hexamethyldisilazane, the modification treatment temperature is 40-60 ℃, and the modification treatment time is 100-140min; the replacement medium is n-hexane, the solvent replacement treatment temperature is 40-50 ℃, and the solvent replacement treatment time is 3-5h;
step two: crushing the aerogel into fine-grain aerogel by adopting an airflow crusher, and then treating the fine-grain aerogel by adopting a spherical shaper to prepare aerogel microbeads;
coating the aerogel microbeads with a coating agent, preparing porous graphite microbeads after drying, curing and carbonizing, mixing silicon powder with the porous graphite microbeads, and sintering in a silicon carbide sintering furnace to obtain hollow silicon carbide microbeads;
the coating agent comprises one of phenolic resin and sucrose solution;
the specific steps of the drying treatment are as follows:
drying by using an air flow dryer, wherein the inlet temperature of the air flow dryer is 240-260 ℃, the outlet temperature of the air flow dryer is 60-80 ℃, and the drying time is 10-40s;
the curing treatment time is 2-4h, and the curing treatment temperature is 120-160 ℃;
the carbonization time is 1-4h, and the carbonization temperature is 400-800 ℃;
the sintering treatment time in a silicon carbide sintering furnace is 2-6h, and the sintering treatment temperature is 1400-2000 ℃;
according to mass percentage, the layered graphene is 2-4%, the silica sol is 10-15%, the ethanol aqueous solution is 5-8%, the ammonia water is 0.06-0.12%, the aging agent is 10-15%, the modifier is 10-15%, the displacing medium is 10-15%, the coating agent is 10-15%, and the silicon powder is 20-30%.
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| CN102718217A (en) * | 2012-05-18 | 2012-10-10 | 湖北大学 | High purity linear silicon carbide powder and preparation method |
| CN112047343A (en) * | 2020-08-25 | 2020-12-08 | 峨眉山市鑫锐新材料有限公司 | Preparation method of hollow silicon carbide microspheres |
| CN114478053A (en) * | 2022-01-30 | 2022-05-13 | 华中科技大学 | Aluminum-based silicon carbide composite material and preparation method thereof |
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| US9728777B2 (en) * | 2013-07-26 | 2017-08-08 | Nanoteck Instruments, Inc. | Methods for mass-producing silicon nano powder and graphene-doped silicon nano powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718217A (en) * | 2012-05-18 | 2012-10-10 | 湖北大学 | High purity linear silicon carbide powder and preparation method |
| CN112047343A (en) * | 2020-08-25 | 2020-12-08 | 峨眉山市鑫锐新材料有限公司 | Preparation method of hollow silicon carbide microspheres |
| CN114478053A (en) * | 2022-01-30 | 2022-05-13 | 华中科技大学 | Aluminum-based silicon carbide composite material and preparation method thereof |
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