CN111825093B - Preparation method of SiC nano powder particles - Google Patents
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Abstract
A preparation method of SiC nano powder particles belongs to the technical field of silicon carbide preparation, ceramic powder and nano material preparation, and aims to solve the problems of low yield, uneven particle size distribution and low purity of the existing silicon carbide powder preparation. The method comprises the following steps: firstly, preparing a macromolecular polysaccharide colloidal solution; secondly, preparing a reaction precursor xerogel powder; thirdly, preparing a primary product of the nano SiC particles; fourthly, regulating and controlling preparation of nano SiC powder particles; and fifthly, removing impurities to finish the preparation of the SiC nano powder particles. The size of the generated SiC particles can be regulated and controlled according to the proportion of reactants and the addition amount of the shape regulator; the SiC nano powder particles prepared by the method have the advantages of nano scale, uniform granularity, high purity, high yield and batch industrial production. The method is applied to the preparation of SiC nano powder particles.
Description
Technical Field
The invention belongs to the technical field of silicon carbide preparation, ceramic powder and nano material preparation, and particularly relates to a preparation method of SiC nano powder particles.
Background
The silicon carbide has the characteristics of large forbidden band width, stable chemical property, strong acid resistance, strong alkali resistance, oxidation resistance, high thermal conductivity, strong thermal stability, high electron saturation mobility, high critical breakdown voltage and the like, and has wide application prospect in the aspects of high-temperature, high-frequency, high-power and anti-irradiation semiconductor devices. The silicon carbide nano powder particle material becomes a research hotspot in the field of materials by the unique physical properties of light, electricity, machinery and the like. The macro-quantitative and large-scale preparation of silicon carbide nanoparticles with uniform nanoscale size is still an important problem in the current industry. Carbothermic reduction using conventional sources of carbon silicon is a commonly used industrial method for the preparation of silicon carbide. Such as carbon black, graphite, silicon dioxide, silicon powder and the like as carbon silicon sources, compared with crystalline solid granular carbon and silicon sources, the sol-state carbon source and the silicon source dispersion system are liquid phases, and the mixing degree is uniform. Because the sol-gel method adopts the compound with high chemical activity component as the precursor to form uniform and stable sol, the preparation of the nano silicon carbide particles is facilitated.
By researching the thermodynamic nucleation and the kinetic growth behavior in the sol-gel method, the growth mechanism for controlling the micro-morphology of the powder is mastered, the bottleneck problem of industrialization of the silicon carbide nano powder is broken through, and the research of the domestic high-end silicon carbide nano powder has important significance.
Disclosure of Invention
The invention aims to solve the problems of low yield, uneven particle size distribution and low purity of the existing preparation of silicon carbide powder, and provides a preparation method of SiC nano powder particles.
A preparation method of SiC nano powder particles is realized according to the following steps:
firstly, preparing a macromolecular polysaccharide colloidal solution:
preparing cetyl trimethyl ammonium bromide into a cationic surfactant solution with the concentration of 0.1-1 mol/L by using deionized water or absolute ethyl alcohol, then sequentially adding alkaline substances, ammonia water and anthraquinone under an ultrasonic dispersion condition, standing for 1-3 h to obtain an alkaline dissolving agent, then adding biomass macromolecular polysaccharide, and stirring for 1-5 h at the rotating speed of 3000-8000 r/min to obtain a macromolecular polysaccharide colloidal solution;
secondly, preparing a reaction precursor xerogel powder:
adding tetraethoxysilane and hexamethyldisilane into the macromolecular polysaccharide colloidal solution obtained in the step one to prepare a precursor solution, then uniformly stirring the precursor solution under constant-temperature heating in a water bath at the temperature of 60-90 ℃ to obtain a gel system, standing and drying the gel system to obtain a dry gel block, and grinding the dry gel block into powder to obtain a reaction precursor dry gel powder; the mass ratio of the macromolecular polysaccharide colloidal solution to the total mass of the ethyl orthosilicate and the hexamethyldisilane is 10: 1;
thirdly, preparing a primary product of the nano SiC particles:
placing the dry gel powder of the reaction precursor obtained in the step two in the center of a covered graphite crucible, and carrying out carbonization treatment under the protection of inert gas to obtain a primary product of nano SiC particles;
fourthly, regulating and preparing the nano SiC powder particles:
uniformly mixing the primary nano SiC particle product obtained in the step three with a shape regulator according to the mass ratio of (10-50): 1, then placing the mixture in the center of a covered graphite crucible, and carrying out sintering reaction under the protection of inert gas to complete the regulation and control of nano SiC powder particles;
fifthly, removing impurities: and (5) removing impurities from the nano SiC powder particles which are regulated and controlled in the fourth step to complete the preparation of the SiC nano powder particles.
The reaction principle of the invention is as follows: the biomass macromolecular polysaccharide is treated and dissolved by an alkaline solution system to be used as a reaction carbon source, and the surfactant is utilized to reduce the surface tension of the alkaline dissolving solution to promote the permeation and accelerate the dissolution of the biomacromoleculeA large amount of active groups are contained in the biomass material, and the active groups are dissolved and then are beneficial to uniformly dispersing with the silicon source in the solution system. Ethyl orthosilicate and hexamethyldisilane are subjected to a series of operations to provide a carbon source and a silicon source in the reaction. In a liquid phase dispersion system by a sol-gel method, the mixing degree of the carbon source and the silicon source is more uniform than that of the solid reaction raw material which is mechanically mixed. In the form of MgCl as a shape regulator2Under the action, the carbon and silicon sources which are completely mixed at high temperature uniformly enter the interior of molten metal salt ions, the growth process of SiC is effectively controlled to grow along the (111) crystal face with the lowest accumulated energy of the silicon carbide crystals, and the supersaturated linear growth is inhibited in the reaction process, so that the preparation of nano-scale particles is realized; and the size of the generated SiC particles can be regulated and controlled according to the proportion of reactants and the addition amount of the shape regulator.
The invention has the beneficial effects that: the prepared SiC nano powder particles have the advantages of nano scale, uniform granularity, high purity, high yield and batch industrial production.
The method is applied to the preparation of SiC nano powder particles.
Drawings
FIG. 1 is an XRD spectrum of SiC nanopowder particles prepared in the examples;
FIG. 2 is a microscopic morphology of SiC nanopowder particles prepared in the examples.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the SiC nano powder particles is realized according to the following steps:
firstly, preparing a macromolecular polysaccharide colloidal solution:
preparing cetyl trimethyl ammonium bromide into a cationic surfactant solution with the concentration of 0.1-1 mol/L by using deionized water or absolute ethyl alcohol, then sequentially adding alkaline substances, ammonia water and anthraquinone under an ultrasonic dispersion condition, standing for 1-3 h to obtain an alkaline dissolving agent, then adding biomass macromolecular polysaccharide, and stirring for 1-5 h at the rotating speed of 3000-8000 r/min to obtain a macromolecular polysaccharide colloidal solution;
secondly, preparing a reaction precursor xerogel powder:
adding tetraethoxysilane and hexamethyldisilane into the macromolecular polysaccharide colloidal solution obtained in the step one to prepare a precursor solution, then uniformly stirring the precursor solution under constant-temperature heating in a water bath at the temperature of 60-90 ℃ to obtain a gel system, standing and drying the gel system to obtain a dry gel block, and grinding the dry gel block into powder to obtain a reaction precursor dry gel powder;
thirdly, preparing a primary product of the nano SiC particles:
placing the dry gel powder of the reaction precursor obtained in the step two in the center of a covered graphite crucible, and carrying out carbonization treatment under the protection of inert gas to obtain a primary product of nano SiC particles;
fourthly, regulating and preparing the nano SiC powder particles:
uniformly mixing the primary nano SiC particle product obtained in the step three with a shape regulator according to the mass ratio of (10-50): 1, then placing the mixture in the center of a covered graphite crucible, and carrying out sintering reaction under the protection of inert gas to complete the regulation and control of nano SiC powder particles;
fifthly, removing impurities: and (4) removing impurities from the nano SiC powder particles regulated and controlled in the fourth step to complete the preparation of the SiC nano powder particles.
The purpose of the impurity removal treatment in this embodiment is to remove carbon, silicon, and salts remaining after the reaction, improve the purity of the product, control the internal oxygen content of the prepared SiC nanoparticles, and promote the C, Si atom ordering.
In the fourth step of the present embodiment, high-speed ball milling is used for mixing.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that in the first step, the mass fraction of the alkaline substance in the alkaline dissolving agent is 1-20 w%, the volume fraction of the ammonia water is 1-10%, and the mass fraction of the anthraquinone is 0.05-1 w%. Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: the difference between this embodiment and the first or second embodiment is that in the first step, the alkaline substance is one or a combination of LiOH, NaOH, and KOH. Other steps and parameters are the same as those in the first or second embodiment.
In the case where the basic substance is a composition in the present embodiment, the respective components are mixed in an arbitrary volume ratio.
The fourth concrete implementation mode: the present embodiment is different from the first to the third embodiments in that, in the first step, the biomass macromolecular polysaccharide is one or a combination of more of plant cellulose, bacterial cellulose, lignin and gelatin. Other steps and parameters are the same as those in one of the first to third embodiments.
In the embodiment, when the biomass macromolecular polysaccharide is a composition, the components are mixed according to any volume ratio.
The fifth concrete implementation mode: the difference between the first embodiment and the fourth embodiment is that the addition amount of the biomass macromolecular polysaccharide in the first step is 5-30 w% of the mass of the alkaline dissolving agent. Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode is as follows: this embodiment is different from one of the first to fifth embodiments in that the mass ratio of the macromolecular polysaccharide colloidal solution to the total mass of tetraethoxysilane and hexamethyldisilane is 10: 1. Other steps and parameters are the same as in one of the first to fifth embodiments.
The seventh embodiment: the embodiment is different from the first to sixth embodiments in that the adding ratio of the tetraethoxysilane and the hexamethyldisilane in the second step is 1ml (1 to 10) ml. Other steps and parameters are the same as those in one of the first to sixth embodiments.
The specific implementation mode is eight: the difference between the first embodiment and the seventh embodiment is that the standing time in the second step is 1-2 h; the drying temperature is 100-160 ℃. Other steps and parameters are the same as those in one of the first to seventh embodiments.
The specific implementation method nine: this embodiment is different from the first to eighth embodiments in that the inert gas in the third and fourth steps is nitrogen gas having a purity of 99.9%. Other steps and parameters are the same as those in one to eight of the embodiments.
The detailed implementation mode is ten: the difference between the present embodiment and one of the first to ninth embodiments is that the temperature of the carbonization treatment in the third step is 500-800 ℃, the time is 1-6 h, and the temperature rise rate is 1-5 ℃/min. Other steps and parameters are the same as those in one of the first to ninth embodiments.
The concrete implementation mode eleven: this embodiment is different from the first to tenth embodiments in that the shape-adjusting agent in the fourth step is MgCl2The purity was analytical grade. Other steps and parameters are the same as in one of the first to tenth embodiments.
The detailed implementation mode is twelve: this embodiment differs from one of the first to eleventh embodiments in that the sintering reaction process in step four: and (3) carrying out high-temperature reaction for 1-4 h at 1400-1700 ℃ in a high-temperature sintering furnace under the protection of argon, and then cooling to room temperature at the temperature rising and falling rate of 2.5-10 ℃/min. Other steps and parameters are the same as those in one of the first to eleventh embodiments.
The specific implementation mode is thirteen: the difference between this embodiment and the first to twelfth embodiment is that, in the fifth step, the process of impurity removal treatment: soaking the regulated nano SiC powder particles in hydrofluoric acid with the mass fraction of 40% for 2-8 h, taking out the nano SiC powder particles, repeatedly washing the nano SiC powder particles with distilled water to be neutral, soaking the nano SiC powder particles in hydrogen peroxide solution with the mass fraction of 10-30% for 1-4 h, soaking the nano SiC powder particles in the distilled water for 2-6 h, filtering and drying the nano SiC powder particles, placing the nano SiC powder particles in a muffle furnace, heating the nano SiC powder particles to 500-800 ℃ in air, firing the nano SiC powder particles for 1-6 h, washing, filtering and drying the nano SiC powder particles, placing the nano SiC powder particles in an oxygen atmosphere with the vacuum degree of 0.06-0.09 MPa and the purity of 99.9% in a near infrared heat source, and heating the nano SiC powder particles for 200-300 ℃ for vacuum treatment for 5-10 h. Other steps and parameters are the same as those in one to twelve embodiments.
The beneficial effects of the present invention are demonstrated by the following examples:
example (b):
a preparation method of SiC nano powder particles is realized according to the following steps:
firstly, preparing a macromolecular polysaccharide colloidal solution:
preparing cetyl trimethyl ammonium bromide into a cationic surfactant solution with the concentration of 0.5mol/L by using absolute ethyl alcohol, then sequentially adding alkaline substances, ammonia water and anthraquinone under the condition of ultrasonic dispersion, standing for 3 hours to obtain an alkaline dissolving agent, then adding biomass macromolecular polysaccharide, and stirring for 1 hour at the rotating speed of 6000r/min to obtain a macromolecular polysaccharide colloidal solution;
secondly, preparing a reaction precursor xerogel powder:
adding tetraethoxysilane and hexamethyldisilane into the macromolecular polysaccharide colloidal solution obtained in the step one to prepare a precursor solution, then uniformly stirring the precursor solution under the constant-temperature heating of a water bath at the temperature of 80 ℃ to obtain a gel system, standing and drying the gel system to obtain a dry gel block, and grinding the dry gel block into powder to obtain a reaction precursor dry gel powder; the mass ratio of the macromolecular polysaccharide colloidal solution to the total amount of the ethyl orthosilicate and the hexamethyldisilane is 10: 1;
thirdly, preparing a primary product of the nano SiC particles:
placing the dry gel powder of the reaction precursor obtained in the step two in the center of a covered graphite crucible, and carrying out carbonization treatment under the protection of inert gas to obtain a primary product of nano SiC particles;
fourthly, regulating and preparing the nano SiC powder particles:
uniformly mixing the primary nano SiC particle product obtained in the step three with a shape regulator according to the mass ratio of 50:1, then placing the mixture in the center of a covered graphite crucible, and carrying out sintering reaction under the protection of inert gas to finish the regulation and control of nano SiC powder particles;
fifthly, removing impurities: and (5) removing impurities from the nano SiC powder particles which are regulated and controlled in the fourth step to complete the preparation of the SiC nano powder particles.
In the first step of this example, the mass fraction of the alkaline substance in the alkaline dissolving agent is 15 w%, the volume fraction of the ammonia water is 5%, and the mass fraction of the anthraquinone is 0.05 w%.
In the first step of this embodiment, the alkaline substance is LiOH.
In the first step of this embodiment, the biomass macromolecular polysaccharide is plant cellulose.
In the first step of this example, the addition amount of the biomass macromolecular polysaccharide is 20 w% of the mass of the alkaline dissolving agent.
In the second step of this example, the adding ratio of tetraethoxysilane and hexamethyldisilane is 1: 1 ml.
The standing time in the step two of the embodiment is 2 hours; the drying temperature was 150 ℃.
In the third and fourth steps of this example, the inert gas was nitrogen with a purity of 99.9%.
In the third step of this embodiment, the temperature of the carbonization treatment is 800 ℃, the time is 4h, and the temperature rise rate is 1 ℃/min.
In the fourth step of this example, the shape modifier is MgCl2The purity was analytical grade.
The sintering reaction process in step four of this example: and (3) carrying out high-temperature reaction for 3h at 1600 ℃ in a high-temperature sintering furnace under the protection of argon, and then cooling to room temperature, wherein the heating and cooling rates are both 5 ℃/min.
In the fifth embodiment, the process of impurity removal processing includes: soaking the regulated nano SiC powder particles in hydrofluoric acid with the mass fraction of 40% for treatment for 6h, taking out the nano SiC powder particles, repeatedly washing the nano SiC powder particles with distilled water to be neutral, soaking the nano SiC powder particles in hydrogen peroxide solution with the mass fraction of 20% for treatment for 4h, soaking the nano SiC powder particles in the distilled water for treatment for 6h, filtering and drying the nano SiC powder particles, placing the nano SiC powder particles in a muffle furnace, heating the nano SiC powder particles to 600 ℃ in air, firing the nano SiC powder particles for 4h, washing, filtering and drying the nano SiC powder particles, placing the nano SiC powder particles in an oxygen atmosphere with the vacuum degree of 0.08MPa and the purity of 99.9%, and performing vacuum treatment for 6h under the heating of a near-infrared heat source at 200 ℃.
The X-ray diffraction (XRD) spectrum of the SiC nanopowder particles prepared in this example is shown in fig. 1, and it can be seen that the diffraction peaks at 35.7 °, 41.4 °, 60.0 °, 71.8 ° and 75.4 ° in the figure correspond to the (111), (200), (220), (311) and (222) crystal planes of β -SiC, respectively; no impurity peak is found, which indicates that the method of the embodiment can successfully prepare the beta-SiC material and the product has high purity.
Fig. 2 shows the micro-morphology of the SiC nanopowder particles prepared in this example, which shows that the SiC nanopowder particles prepared in this example have uniform particle size distribution and an average size of 80 nm.
Claims (8)
1. A preparation method of SiC nano powder particles is characterized by comprising the following steps:
firstly, preparing a macromolecular polysaccharide colloidal solution:
preparing cetyl trimethyl ammonium bromide into a cationic surfactant solution with the concentration of 0.1-1 mol/L by using deionized water or absolute ethyl alcohol, then sequentially adding alkaline substances, ammonia water and anthraquinone under an ultrasonic dispersion condition, standing for 1-3 h to obtain an alkaline dissolving agent, then adding biomass macromolecular polysaccharide, and stirring for 1-5 h at the rotating speed of 3000-8000 r/min to obtain a macromolecular polysaccharide colloidal solution;
secondly, preparing dry gel powder of a reaction precursor:
adding tetraethoxysilane and hexamethyldisilane into the macromolecular polysaccharide colloidal solution obtained in the step one to prepare a precursor solution, then uniformly stirring the precursor solution under constant-temperature heating in a water bath at the temperature of 60-90 ℃ to obtain a gel system, standing and drying the gel system to obtain a dry gel block, and grinding the dry gel block into powder to obtain a reaction precursor dry gel powder; the mass ratio of the macromolecular polysaccharide colloidal solution to the total mass of the ethyl orthosilicate and the hexamethyldisilane is 10: 1;
thirdly, preparing a primary product of the nano SiC particles:
placing the dry gel powder of the reaction precursor obtained in the step two in the center of a covered graphite crucible, and carrying out carbonization treatment under the protection of inert gas to obtain a primary product of nano SiC particles;
fourthly, regulating and preparing the nano SiC powder particles:
uniformly mixing the primary nano SiC particle product obtained in the step three with a shape regulator according to the mass ratio of (10-50): 1, then placing the mixture in the center of a covered graphite crucible, and carrying out sintering reaction under the protection of inert gas to complete the regulation and control of nano SiC powder particles;
fifthly, removing impurities: carrying out impurity removal treatment on the nano SiC powder particles subjected to regulation and control in the fourth step to complete preparation of the SiC nano powder particles;
wherein the shape regulator in the fourth step is MgCl2The purity is analytically pure;
the sintering reaction process in the fourth step: and (3) carrying out high-temperature reaction for 3h at 1600 ℃ in a high-temperature sintering furnace under the protection of argon, and then cooling to room temperature, wherein the heating and cooling rates are both 5 ℃/min.
2. The method for preparing SiC nano powder particles according to claim 1, wherein in the first step, the mass fraction of the alkaline substance in the alkaline dissolving agent is 1-20 w%, the volume fraction of the ammonia water is 1-10 w%, and the mass fraction of the anthraquinone is 0.05-1 w%.
3. The method of claim 1, wherein the alkaline substance is one or more of LiOH, NaOH, and KOH.
4. The method for preparing SiC nano powder particles according to claim 1, wherein in the first step, the biomass macromolecular polysaccharide is one or a combination of more of plant cellulose, bacterial cellulose, lignin and gelatin.
5. The method for preparing SiC nano powder particles according to claim 1, wherein the addition amount of the biomass macromolecular polysaccharide in the first step is 5-30 w% of the mass of the alkaline dissolving agent.
6. The method for preparing SiC nano powder particles according to claim 1, wherein the adding proportion of the tetraethoxysilane and the hexamethyldisilane in the step two is 1ml (1-10) ml; the standing time is 1-2 h; the drying temperature is 100-160 ℃.
7. The method for preparing SiC nano powder particles according to claim 1, wherein the temperature of the carbonization treatment in the third step is 500-800 ℃, the time is 1-6 h, and the temperature rise rate is 1-5 ℃/min.
8. The method for preparing SiC nano powder particles according to claim 1, wherein the impurity removal treatment in the fifth step comprises: soaking the regulated nano SiC powder particles in hydrofluoric acid with the mass fraction of 40% for 2-8 h, taking out the nano SiC powder particles, repeatedly washing the nano SiC powder particles with distilled water to be neutral, soaking the nano SiC powder particles in hydrogen peroxide solution with the mass fraction of 10-30% for 1-4 h, soaking the nano SiC powder particles in the distilled water for 2-6 h, filtering and drying the nano SiC powder particles, placing the nano SiC powder particles in a muffle furnace, heating the nano SiC powder particles to 500-800 ℃ in air, firing the nano SiC powder particles for 1-6 h, washing, filtering and drying the nano SiC powder particles, placing the nano SiC powder particles in an oxygen atmosphere with the vacuum degree of 0.06-0.09 MPa and the purity of 99.9% in a near infrared heat source, and heating the nano SiC powder particles for 200-300 ℃ for vacuum treatment for 5-10 h.
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