CN109607540B - Process for preparing nano silicon carbide by sol-gel method - Google Patents
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- CN109607540B CN109607540B CN201910094856.2A CN201910094856A CN109607540B CN 109607540 B CN109607540 B CN 109607540B CN 201910094856 A CN201910094856 A CN 201910094856A CN 109607540 B CN109607540 B CN 109607540B
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- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/97—Preparation from SiO or SiO2
Abstract
The invention provides a process for preparing nano silicon carbide by using a sol-gel method, and relates to the technical field of preparation of silicon carbide. The method comprises the following steps: s1: preparing silicon dioxide by a sol-gel method; s2: the silicon dioxide prepared in the step S1 is mixed with a homogenizing agent, a carbon source and a combustion-supporting reducing agent in a homogenizing way; s3: reducing at high temperature; s4: and (5) dispersing and grading. According to the invention, the silicon dioxide is prepared by a sol-gel method, and the prepared silicon dioxide is good in dispersion; the silicon carbide prepared by high-temperature reduction after the monodisperse silicon dioxide is uniformly mixed with the homogenizing agent, the carbon source and the combustion-supporting reducing agent has good dispersibility, and the problems of agglomeration and the like in the preparation process of the nano silicon carbide are solved. The reaction energy is activated by the combustion-supporting reducing agent, and the reaction energy barrier is reduced, so that the reduction temperature of silicon dioxide is reduced, and the growth of high-temperature silicon carbide particles is prevented. The carbon source and the monodisperse silicon dioxide are uniformly mixed, so that the reaction process is reduced, and the reduction reaction speed is improved.
Description
Technical Field
The invention relates to the technical field of preparation of silicon carbide, in particular to a process for preparing nano silicon carbide by using a sol-gel method.
Background
Silicon carbide has many excellent physical and chemical properties, such as high hardness, high strength, stable chemical properties, good high temperature oxidation resistance, etc. And the material has better chemical compatibility with a plurality of metals and metal oxides, can be used for preparing metal-based, ceramic-based and polymer-based composite materials, plays roles of strengthening, toughening and hardening in the composite materials, can also be directly used as a grinding material or prepared into a grinding tool with a certain shape, and is used for grinding and polishing the surfaces of metals, ceramics, glass, stones and the like.
In recent years, with the development of electronics and computer industries, the demand for single crystal silicon oxide wafers has been increasing, and high quality single crystal silicon wafers must be processed using high quality ultrafine powders such as silicon carbide, and nano-scale silicon carbide has attracted more and more attention. The nano silicon carbide has more unique excellent performances and wider application prospect due to the self micro morphology and the crystal structure, and is generally considered to be expected to become an important component unit of a third-generation wide-band-gap semiconductor material.
In the prior art, a sand mill or an air flow mill is mainly adopted for preparing the nano silicon carbide for physical crushing processing, and in the process of preparing the silicon carbide nano material, the technical problems that a carbon source and a silicon source are difficult to uniformly mix and disperse exist.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a process for preparing nano silicon carbide by using a sol-gel method, which solves the technical problems that a carbon source and a silicon source are difficult to uniformly mix and disperse in the process of preparing a silicon carbide nano material.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a process for preparing nano silicon carbide by using a sol-gel method comprises the following steps:
s1: preparing silicon dioxide by a sol-gel method;
s2: the silicon dioxide prepared in the step S1 is mixed with a homogenizing agent, a carbon source and a combustion-supporting reducing agent in a homogenizing way;
s3: reducing at high temperature;
s4: and (5) dispersing and grading.
Preferably, the specific steps of step S1 are as follows:
s1-1, mixing 1 part of ammonia water, 2 parts of ethanol and 10 parts of distilled water to obtain a solution A;
s1-2, mixing 1 part of ethyl orthosilicate, 10 parts of ethanol and 5 parts of distilled water to obtain a solution B;
s1-3, adding the solution B into the solution A to react for 12 hours;
and S1-4, washing to obtain silicon dioxide.
Preferably, the specific steps of step S2 are as follows:
s2-1, dispersing the silicon dioxide obtained in the step S1 in a liquid phase medium, adding a dispersing agent, and performing ultrasonic stirring to obtain a dispersion liquid;
s2-2, adding a homogenizing agent, a carbon source and a sintering aid reducing agent into the dispersion liquid obtained in the step S2-1;
s2-3. the S2-2 mixture is spin-dried.
Preferably, the specific conditions of step S3 are: and (3) carrying out the sintering in a protective atmosphere, introducing hydrogen, wherein the sintering temperature is 800-1600 ℃, and the sintering heat preservation time is 4-10 h.
Preferably, the specific steps of step S4 are as follows: and (3) performing grading treatment by airflow milling under a nitrogen protective atmosphere.
Preferably, the dispersant in step S2-1 is one or more of an aqueous dispersant and an oily dispersant.
Preferably, in the step S2-2, the homogenizing agent is NaCl, KCl, ZnCl2And LiCl.
Preferably, in step S2-2, the combustion-supporting reducing agent is: one or more of magnesium, carbon and potassium; the carbon source substances are: one or more of resin, glucose, fatty acid, petroleum, peanut and pressed powder.
Preferably, in step S2-3, the spin drying conditions are: the drying temperature is 40-100 ℃, and the drying time is 2-10 h.
Preferably, in the step S3, the protective atmosphere is nitrogen or argon, the pressure is micro-positive pressure, and the introduction amount of hydrogen is 10 to 200mL/min
(III) advantageous effects
The invention provides a process for preparing nano silicon carbide by using a sol-gel method. Compared with the prior art, the method has the following beneficial effects:
according to the invention, the silicon dioxide is prepared by a sol-gel method, and the prepared silicon dioxide is good in dispersion; the silicon carbide prepared by high-temperature reduction after the monodisperse silicon dioxide is uniformly mixed with the homogenizing agent, the carbon source and the combustion-supporting reducing agent has good dispersibility, and the problems of agglomeration and the like in the preparation process of the nano silicon carbide are solved. The reaction energy is activated by the combustion-supporting reducing agent, and the reaction energy barrier is reduced, so that the reduction temperature of silicon dioxide is reduced, and the growth of high-temperature silicon carbide particles is prevented. The carbon source and the monodisperse silicon dioxide are uniformly mixed, so that the reaction process is reduced, and the reduction reaction speed is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of silica particles prepared by a sol-gel process.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the application provides a process for preparing nano silicon carbide by using a sol-gel method, and solves the technical problems that a carbon source and a silicon source are difficult to uniformly mix and disperse in the process of preparing a silicon carbide nano material. The mixing degree of the carbon source and the silicon source is improved.
In order to solve the problem of crosstalk, the technical scheme in the embodiment of the present application has the following general idea:
the silicon carbide powder prepared by the preparation of the silicon dioxide by the sol-gel method and the homogeneous mixing, the high-temperature reduction and the dispersion grading has narrow particle size distribution and high purity.
In order to better understand the technical solution, the technical solution will be described in detail with reference to the drawings and the specific embodiments.
The embodiment of the invention provides a process for preparing nano silicon carbide by using a sol-gel method, which comprises the following steps:
s1: preparing silicon dioxide by a sol-gel method;
s2: the silicon dioxide prepared in the step S1 is mixed with a homogenizing agent, a carbon source and a sintering aid reducing agent in a homogenizing way;
s3: reducing at high temperature;
s4: and (5) dispersing and grading.
According to the invention, the silicon dioxide is prepared by a sol-gel method, and the prepared silicon dioxide is good in dispersion; the silicon carbide prepared by high-temperature reduction after the monodisperse silicon dioxide is uniformly mixed with the homogenizing agent, the carbon source and the combustion-supporting reducing agent has good dispersibility, and the problems of agglomeration and the like in the preparation process of the nano silicon carbide are solved. The reaction energy is activated by the combustion-supporting reducing agent, and the reaction energy barrier is reduced, so that the reduction temperature of silicon dioxide is reduced, and the growth of high-temperature silicon carbide particles is prevented. The carbon source and the monodisperse silicon dioxide are uniformly mixed, so that the reaction process is reduced, and the reduction reaction speed is improved.
In a specific implementation process, the specific steps of step S1 are as follows:
s1-1, stirring 1 part of ammonia water and 2 parts of ethanol in a container, and distilling 10 parts of ethanol to prepare solution A;
s1-2, stirring the following solvents in a container: preparing a solution B from 1 part of ethyl orthosilicate, 10 parts of ethanol and 5 parts of distilled water;
s1-3, adding the solution B into the solution A to react for 12 hours;
and S1-4, washing to obtain silicon dioxide.
The specific raw material components of the S1-1 and the S1-2 are in volume ratio.
As shown in FIG. 1, which is a schematic diagram of silica particles prepared by a sol-gel method, it can be seen that the silica particles are highly dispersed single particles with a particle size of 200-500 nm, and have good dispersibility.
In a specific implementation process, the specific steps of step S2 are as follows:
s2-1, dispersing the silicon dioxide obtained in the step S1 in a liquid phase medium, adding a dispersing agent, and performing ultrasonic stirring to obtain a dispersion liquid;
s2-2, adding a homogenizing agent, a carbon source and a sintering aid reducing agent into the dispersion liquid obtained in the step S2-1;
s2-3. the S2-2 mixture is spin-dried.
In a specific implementation process, the specific conditions of step S3 are as follows: and (3) carrying out the sintering in a protective atmosphere, introducing hydrogen, wherein the sintering temperature is 800-1600 ℃, and the sintering heat preservation time is 4-10 h.
In a specific implementation process, the specific steps of step S4 are as follows: and (3) performing grading treatment by airflow milling under a nitrogen protective atmosphere.
In a specific implementation process, the dispersant in the step S2-1 is one or more of an aqueous dispersant and an oily dispersant. Specifically, the dispersant may be one or more of a polymer LBD-1 dispersant, a dispersant NNO, a dispersant MF, sodium lignosulfonate, acetone, alcohol, PAN and the like.
In the specific implementation process, in the step S2-2, the homogenizing agent is NaCl, KCl or ZnCl2And LiCl.
In a specific implementation process, in the step S2-2, the combustion-supporting reducing agent is: one or more of magnesium, carbon and potassium; the carbon source substances are: one or more of resin, glucose, fatty acid, petroleum, peanut and pressed powder.
In a specific implementation process, in the step S2-3, the conditions of spin drying are as follows: the drying temperature is 40-100 ℃, and the drying time is 2-10 h.
In the specific implementation process, in the step S3, the protective atmosphere is nitrogen or argon, the pressure is micro-positive pressure, and the introduction amount of hydrogen is 10 to 200 mL/min.
The following is a detailed description of the specific examples:
example 1:
a process for preparing nano silicon carbide by using a sol-gel method comprises the following steps:
s1: preparing silicon dioxide by a sol-gel method;
s1-1, mixing 1 part of ammonia water, 2 parts of ethanol and 10 parts of distilled water to obtain a solution A;
s1-2, mixing 1 part of ethyl orthosilicate, 10 parts of ethanol and 5 parts of distilled water to obtain a solution B;
s1-3, adding the solution B into the solution A to react for 12 hours;
and S1-4, washing to obtain silicon dioxide.
S2: the silicon dioxide prepared in the step S1 is mixed with a homogenizing agent, a carbon source and a combustion-supporting reducing agent in a homogenizing way;
s2-1, dispersing the silicon dioxide obtained in the step S1 in a liquid phase medium, adding a dispersing agent, and performing ultrasonic stirring to obtain a dispersion liquid; the dispersant is one or more of aqueous dispersant and oily dispersant. The homogenizing agent is NaCl, KCl, ZnCl2And LiCl.
S2-2, adding a homogenizing agent, a carbon source and a sintering aid reducing agent into the dispersion liquid obtained in the step S2-1; the combustion-supporting reducing agent is as follows: one or more of magnesium, carbon and potassium; the carbon source substances are: one or more of resin, glucose, fatty acid, petroleum, peanut and pressed powder.
S2-3. the S2-2 mixture is spin-dried. The conditions of the rotary drying are as follows: the drying temperature is 40 ℃ and the drying time is 2 h.
S3: reducing at high temperature;
the preparation method is carried out in a protective atmosphere, hydrogen is introduced, the sintering temperature is 800 ℃, and the sintering heat preservation time is 4 hours. The protective atmosphere is nitrogen or argon, the pressure is micro-positive pressure, and the introduction amount of hydrogen is 10 mL/min.
S4: and (3) performing grading treatment by airflow milling under a nitrogen protective atmosphere.
Example 2:
a process for preparing nano silicon carbide by using a sol-gel method comprises the following steps:
s1: preparing silicon dioxide by a sol-gel method;
s1-1, mixing 1 part of ammonia water, 2 parts of ethanol and 10 parts of distilled water to obtain a solution A;
s1-2, mixing 1 part of ethyl orthosilicate, 10 parts of ethanol and 5 parts of distilled water to obtain a solution B;
s1-3, adding the solution B into the solution A to react for 12 hours;
and S1-4, washing to obtain silicon dioxide.
S2: the silicon dioxide prepared in the step S1 is mixed with a homogenizing agent, a carbon source and a combustion-supporting reducing agent in a homogenizing way;
s2-1, dispersing the silicon dioxide obtained in the step S1 in a liquid phase medium, adding a dispersing agent, and performing ultrasonic stirring to obtain a dispersion liquid; the dispersant is one or more of aqueous dispersant and oily dispersant. The homogenizing agent is NaCl, KCl, ZnCl2And LiCl.
S2-2, adding a homogenizing agent, a carbon source and a sintering aid reducing agent into the dispersion liquid obtained in the step S2-1; the combustion-supporting reducing agent is as follows: one or more of magnesium, carbon and potassium; the carbon source substances are: one or more of resin, glucose, fatty acid, petroleum, peanut and pressed powder.
S2-3. the S2-2 mixture is spin-dried. The conditions of the rotary drying are as follows: the drying temperature is 100 ℃ and the drying time is 10 h.
S3: reducing at high temperature;
the preparation method is carried out in a protective atmosphere, hydrogen is introduced, the sintering temperature is 1600 ℃, and the sintering heat preservation time is 10 hours. The protective atmosphere is nitrogen or argon, the pressure is micro-positive pressure, and the introduction amount of hydrogen is 200 mL/min.
S4: and (3) performing grading treatment by airflow milling under a nitrogen protective atmosphere.
Example 3:
a process for preparing nano silicon carbide by using a sol-gel method comprises the following steps:
s1: preparing silicon dioxide by a sol-gel method;
s1-1, mixing 1 part of ammonia water, 2 parts of ethanol and 10 parts of distilled water to obtain a solution A;
s1-2, mixing 1 part of ethyl orthosilicate, 10 parts of ethanol and 5 parts of distilled water to obtain a solution B;
s1-3, adding the solution B into the solution A to react for 12 hours;
and S1-4, washing to obtain silicon dioxide.
S2: the silicon dioxide prepared in the step S1 is mixed with a homogenizing agent, a carbon source and a combustion-supporting reducing agent in a homogenizing way;
s2-1, dispersing the silicon dioxide obtained in the step S1 in a liquid phase medium, adding a dispersing agent, and performing ultrasonic stirring to obtain a dispersion liquid; the dispersant is one or more of aqueous dispersant and oily dispersant. The homogenizing agent is NaCl, KCl, ZnCl2And LiCl.
S2-2, adding a homogenizing agent, a carbon source and a sintering aid reducing agent into the dispersion liquid obtained in the step S2-1; the combustion-supporting reducing agent is as follows: one or more of magnesium, carbon and potassium; the carbon source substances are: one or more of resin, glucose, fatty acid, petroleum, peanut and pressed powder.
S2-3. the S2-2 mixture is spin-dried. The conditions of the rotary drying are as follows: the drying temperature is 70 ℃ and the drying time is 6 h.
S3: reducing at high temperature;
the preparation method is carried out in a protective atmosphere, hydrogen is introduced, the sintering temperature is 1200 ℃, and the sintering heat preservation time is 7 hours. The protective atmosphere is nitrogen or argon, the pressure is micro-positive pressure, and the introduction amount of hydrogen is 110 mL/min.
S4: and (3) performing grading treatment by airflow milling under a nitrogen protective atmosphere.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. A process for preparing nano silicon carbide by using a sol-gel method is characterized by comprising the following steps:
s1: preparing silicon dioxide by a sol-gel method;
s2: the silicon dioxide prepared in the step S1 is mixed with a homogenizing agent, a carbon source and a combustion-supporting reducing agent in a homogenizing way;
s3: reducing at high temperature;
s4: dispersing and grading;
the specific steps of step S1 are as follows:
s1-1, mixing 1 part of ammonia water, 2 parts of ethanol and 10 parts of distilled water to obtain a solution A;
s1-2, mixing 1 part of ethyl orthosilicate, 10 parts of ethanol and 5 parts of distilled water to obtain a solution B;
s1-3, adding the solution B into the solution A to react for 12 hours;
s1-4, washing to obtain silicon dioxide;
the specific steps of step S2 are as follows:
s2-1, dispersing the silicon dioxide obtained in the step S1 in a liquid phase medium, adding a dispersing agent, and performing ultrasonic stirring to obtain a dispersion liquid;
s2-2, adding a homogenizing agent, a carbon source and a sintering aid reducing agent into the dispersion liquid obtained in the step S2-1;
s2-3, carrying out rotary drying on the S2-2 mixture;
specific conditions of the step S3 are as follows: the sintering is carried out in a protective atmosphere, hydrogen is introduced, the sintering temperature is 1200-1600 ℃, and the sintering heat preservation time is 4-10 hours;
in the step S2-2, the homogenizing agent is NaCl, KCl, ZnCl2One or more of LiCl;
in the step S2-2, the combustion-supporting reducing agent is: one or more of magnesium, carbon and potassium; the carbon source substances are: one or more of resin, glucose, fatty acid, petroleum, peanut and pressed powder.
2. The process for preparing nano silicon carbide according to claim 1, wherein the step S4 comprises the following steps: and (3) performing grading treatment by airflow milling under a nitrogen protective atmosphere.
3. The process for preparing nano silicon carbide according to claim 1, wherein the dispersant in step S2-1 is one or more of an aqueous dispersant and an oily dispersant.
4. The process for preparing nano silicon carbide according to the sol-gel method of claim 1, wherein in the step S2-3, the conditions of the spin drying are as follows: the drying temperature is 40-100 ℃, and the drying time is 2-10 h.
5. The process for preparing nano silicon carbide according to claim 1, wherein in the step S3, the protective atmosphere is nitrogen or argon, the pressure is micro positive pressure, and the introduction amount of hydrogen is 10 to 200 mL/min.
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