CN114835124B - Preparation method of nano silicon carbide particles based on ferric nitrate shape regulator - Google Patents
Preparation method of nano silicon carbide particles based on ferric nitrate shape regulator Download PDFInfo
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- CN114835124B CN114835124B CN202210570209.6A CN202210570209A CN114835124B CN 114835124 B CN114835124 B CN 114835124B CN 202210570209 A CN202210570209 A CN 202210570209A CN 114835124 B CN114835124 B CN 114835124B
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 title claims abstract description 70
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 41
- 239000002245 particle Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 239000007833 carbon precursor Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000012686 silicon precursor Substances 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 12
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 12
- -1 polydimethylsiloxane Polymers 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000005011 phenolic resin Substances 0.000 claims description 10
- 229920001568 phenolic resin Polymers 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 2
- 239000003607 modifier Substances 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 20
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B32/977—Preparation from organic compounds containing silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A preparation method of nano silicon carbide particles based on ferric nitrate shape regulator belongs to the technical field of silicon carbide powder preparation, and aims to solve the problems of complex preparation process, low yield and uneven morphology and granularity of the existing silicon carbide powder. The method comprises the following steps: 1. preparing silicon and carbon precursor powder; 2. and after sintering and impurity removal, obtaining the nano silicon carbide particles based on the ferric nitrate shape regulator. According to the invention, ferric nitrate is used as a shape regulator, and the obtained nano silicon carbide particles based on the ferric nitrate shape regulator are uniform in particle size distribution. The solvent components such as water and the like are not introduced in the whole preparation process, reactants are introduced in a solid form, the reaction process is easy to control, the product purity is high, the process is simple, the yield is improved, and the method is suitable for industrial production. The unique combination of the carbon source, the silicon source precursor and the ferric nitrate provides a material basis for the micro-morphology adjustment of the silicon carbide. The method is suitable for preparing the nano silicon carbide particles based on the ferric nitrate shape regulator.
Description
Technical Field
The invention belongs to the technical field of preparation of silicon carbide powder, and particularly relates to a preparation method of nano silicon carbide particles based on an iron nitrate shape regulator.
Background
Ceramic materials are irreplaceable materials in various fields due to excellent mechanical properties and high-temperature stability, wherein innovation of preparation technology of ceramic powder has important significance for development of ceramic materials. Silicon carbide has the excellent characteristics of light weight, high hardness, high strength, acid and alkali resistance, high temperature resistance and the like. The particle reinforced ceramic is a reinforced or toughened ceramic matrix composite material obtained by introducing particles as a second phase reinforcing phase into a ceramic matrix, uniformly dispersing and distributing the particles and compositing the particles with the matrix, and the silicon carbide particles are required to have the characteristic of uniform size and regular morphology. The preparation of the silicon carbide particle powder with uniform size has the problems of low product purity, reduced yield, unstable product size, uneven particle size distribution and the like. Therefore, the method has great significance for the research on the preparation of nano-scale silicon carbide particle powder.
Disclosure of Invention
The invention aims to solve the problems of complex preparation process, low yield and uneven morphology and granularity of the existing silicon carbide powder, and provides a preparation method of nano silicon carbide particles based on an iron nitrate shape regulator.
The preparation method of the nano silicon carbide particles based on the ferric nitrate shape regulator comprises the following steps:
1. preparation of silicon, carbon precursor powder:
uniformly mixing polydimethylsiloxane and a curing agent, curing, then carbonizing, and adding carbonized products, phenolic resin powder and ferric nitrate powder into a high-speed mixer together for processing to obtain silicon and carbon precursor powder;
2. sintering and removing impurities:
placing the silicon and carbon precursor powder into a graphite crucible, placing the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1250-1600 ℃, reacting for 5-10 hours to obtain an initial product, and removing impurities to obtain nano silicon carbide particles based on an iron nitrate shape regulator, thereby completing the preparation method;
the mass ratio of the polydimethylsiloxane to the curing agent is 9:1;
the carbonization treatment comprises the following steps: raising the temperature to 800 ℃ at the speed of 1-3.5 ℃/min, and preserving the heat for 2-5 h;
the mass ratio of the carbonized product to the phenolic resin powder to the ferric nitrate powder is (1-50): 1;
parameters of the high-speed mixer: mixing for 5-10 h at a rotating speed of 60-100 r/min under the power of 1-20 Hz;
the purity of the argon is 99.99 percent;
the temperature in the high-temperature sintering furnace is raised to 800 ℃ at a speed of 1-3.5 ℃/min, the temperature is kept for 2-5 h, then the temperature is continuously raised to 1250-1600 ℃ at a speed of 2-5 ℃/min, the temperature is kept for 5-10 h, and the cooling rate and the heating rate after the temperature is kept the same;
the impurity removal treatment; and (3) placing the initial product in a muffle furnace, heating to 600-800 ℃ under air, and burning for 1-6 h.
The reaction principle of the invention is as follows: adopts a novel carbon source and silicon source combination and a double-carbon source reaction system. Under the combined action of ferric nitrate powder and the novel carbon source and silicon source precursor, the carbon source and the silicon source are regulated and controlled to react in a molten state so as to realize the growth of low-size nanowire silicon carbide particles. The existence of the shape regulator metal salt inhibits the current growth of silicon carbide grains in the growth process, thereby forming a spheroidal morphology.
The beneficial effects of the invention are as follows: the nano silicon carbide particles based on the ferric nitrate shape regulator are prepared by adopting the ferric nitrate as the shape regulator, and have uniform particle size distribution and nano-scale average size. The invention has the advantages that solvent components such as water are not introduced in the whole preparation process, reactants are introduced in a solid form, the reaction process is easy to control, the product purity is high, the preparation process is simple, the yield is improved, and the invention is suitable for industrial production. The unique combination of the carbon source, the silicon source precursor and the ferric nitrate provides a material basis for the micro-morphology adjustment of the silicon carbide.
The method is suitable for preparing the nano silicon carbide particles based on the ferric nitrate shape regulator.
Drawings
FIG. 1 is an XRD spectrum of nano-sized silicon carbide particles based on a ferric nitrate shape adjuster prepared in the example;
fig. 2 is a TEM image of the resulting nano-silicon carbide particles based on the ferric nitrate shape adjuster prepared in the example.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and also includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the nano silicon carbide particles based on the ferric nitrate shape regulator is realized by the following steps:
1. preparation of silicon, carbon precursor powder:
uniformly mixing polydimethylsiloxane and a curing agent, curing, then carbonizing, and adding carbonized products, phenolic resin powder and ferric nitrate powder into a high-speed mixer together for processing to obtain silicon and carbon precursor powder;
2. sintering and removing impurities:
the silicon and carbon precursor powder is placed into a graphite crucible, placed into a high-temperature sintering furnace under the protection of argon, heated to 1250-1600 ℃, reacted for 5-10 hours to obtain an initial product, and subjected to impurity removal treatment to obtain nano silicon carbide particles based on an iron nitrate shape regulator, thus the preparation method is completed.
In the first embodiment, the polydimethylsiloxane and the curing agent are commercial products, and specific curing conditions are operated according to the specification of the commercial products.
In the first embodiment, the treatment is performed in a high-speed mixer by pulverizing and grinding the block and uniformly mixing the block with the powder.
In the second embodiment, the impurity removal treatment is directly performed to ensure that the carbon component is excessive in the reaction process, so that a dual-carbon source reaction system is adopted in the raw material proportion of the first embodiment, and the initial product is excessive carbon after the reaction time is ensured.
In the first embodiment, the polydimethylsiloxane is used as a carbon source and a silicon source together, and the phenolic resin is used as a supplementary carbon source.
The second embodiment is as follows: the first embodiment is different from the second embodiment in that the mass ratio of the polydimethylsiloxane to the curing agent in the first step is 9:1. Other steps and parameters are the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiments in that the carbonization treatment is described in the first step: raising the temperature to 800 ℃ at the speed of 1-3.5 ℃/min, and preserving the heat for 2-5 h. Other steps and parameters are the same as in the first or second embodiment.
The specific embodiment IV is as follows: this embodiment differs from one to three embodiments in that the mass ratio of the carbonized product, the phenolic resin powder, and the ferric nitrate powder in the step one is (1 to 50): 1. Other steps and parameters are the same as in one to three embodiments.
Fifth embodiment: this embodiment differs from one to four embodiments in the parameters of the high speed mixer described in step one: mixing for 5-10 h at the rotating speed of 60-100 r/min under the power of 1-20 Hz. Other steps and parameters are the same as in one to four embodiments.
Specific embodiment six: this embodiment differs from one of the first to fifth embodiments in that the purity of the argon gas in the second step is 99.99%. Other steps and parameters are the same as in one of the first to fifth embodiments.
Seventh embodiment: the difference between the embodiment and one of the first to sixth embodiments is that in the step two, the temperature in the high-temperature sintering furnace is raised to 800 ℃ at a speed of 1 to 3.5 ℃/min, the temperature is kept for 2 to 5 hours, then the temperature is continuously raised to 1250 to 1600 ℃ at a speed of 2 to 5 ℃/min, the temperature is kept for 5 to 10 hours, and the cooling rate and the heating rate after the completion are kept the same. Other steps and parameters are the same as in one of the first to sixth embodiments.
In the embodiment, the purpose of heat preservation at 800 ℃ for 2-5 hours is to carbonize the organic carbon component, and the generated elemental carbon participates in the subsequent generation of silicon carbide.
Eighth embodiment: the present embodiment is different from one of the first to seventh embodiments in that the impurity removal treatment is described in the second step; and (3) placing the initial product in a muffle furnace, heating to 600-800 ℃ under air, and burning for 1-6 h. Other steps and parameters are the same as those of one of the first to seventh embodiments.
The beneficial effects of the invention are verified by the following examples:
examples:
the preparation method of the nano silicon carbide particles based on the ferric nitrate shape regulator comprises the following steps:
1. preparation of silicon, carbon precursor powder:
uniformly mixing polydimethylsiloxane and a curing agent, curing, then carbonizing, and adding carbonized products, phenolic resin powder and ferric nitrate powder into a high-speed mixer together for processing to obtain silicon and carbon precursor powder;
2. sintering and removing impurities:
placing the silicon and carbon precursor powder into a graphite crucible, placing the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1250-1600 ℃, reacting for 5-10 hours to obtain an initial product, and removing impurities to obtain nano silicon carbide particles based on an iron nitrate shape regulator, thereby completing the preparation method;
the mass ratio of the polydimethylsiloxane to the curing agent is 9:1;
the carbonization treatment comprises the following steps: heating to 800 ℃ at a speed of 2 ℃/min, and preserving heat for 3 hours;
the mass ratio of the carbonized product to the phenolic resin powder to the ferric nitrate powder is 20:10:1;
parameters of the high-speed mixer: mixing for 8 hours at a rotating speed of 100r/min under the power of 20 Hz;
the purity of the argon is 99.99 percent;
the temperature in the high-temperature sintering furnace is raised to 800 ℃ at a speed of ℃/min, the temperature is kept for 4 hours, then the temperature is continuously raised to 1500 ℃ at a speed of 2.5 ℃/min, the temperature is kept for 5 hours, and the cooling rate and the heating rate after the temperature is kept the same; wherein the purpose of heat preservation for 4 hours at 800 ℃ is to carbonize the organic carbon component, and the generated elemental carbon participates in the generation of subsequent silicon carbide;
the impurity removal treatment; placing the initial product in a muffle furnace, heating to 700 ℃ under air, and burning for 4 hours; the reason for directly carrying out the carbon removal treatment in the impurity removal treatment is to ensure that the carbon component is excessive in the reaction process, so that a double-carbon source reaction system is adopted in the raw material proportion of the first step, and the initial product is excessive carbon after the reaction time.
In the first embodiment, the polydimethylsiloxane and the curing agent are commercial products, and specific curing conditions are operated according to the specification of the commercial products.
The treatment in the high-speed mixer in the first step of this embodiment is to grind the block and mix it with the powder uniformly.
In the first embodiment, the polydimethylsiloxane is used as a carbon source and a silicon source together, and the phenolic resin is used as a supplementary carbon source. In order to ensure the growth of nano-sized morphology silicon carbide particles and effectively inhibit supersaturated linear growth of silicon carbide, ferric nitrate is introduced as a shape regulator.
In this example, the reaction of the carbon source and the silicon source to form silicon carbide is performed at a high temperature under the action of ferric nitrate. The carbon source and the silicon source are complex in system, so that the reaction is performed mainly by ferric nitrate. In the molten state, the ferric nitrate is favorable for promoting the reaction of a silicon source and a carbon source, and the present growth of silicon carbide crystal grains is inhibited in the growth process due to the existence of the metal salt of the shape regulator, so that a spheroidal morphology is formed.
The X-ray diffraction (XRD) spectra of the nano silicon carbide particles based on the ferric nitrate shape regulator prepared in this example are shown in fig. 1, and it can be seen that diffraction peaks at 35.7 °, 41.4 °, 60.0 °, 71.8 ° and 75.4 ° in the figures correspond to (111), (200), (220), (311) and (222) crystal planes of β -SiC, respectively; no impurity peaks were found, indicating that the method in this example was successful in preparing beta-SiC material and that the product purity was high.
The micro morphology of the nano silicon carbide particles based on the ferric nitrate shape regulator prepared in the embodiment is as shown in fig. 2, the nano spherical micro morphology of the silicon carbide particles prepared based on the method of the invention in the embodiment is uniform in morphology and particle size distribution.
Claims (3)
1. The preparation method of the nano silicon carbide particles based on the ferric nitrate shape regulator is characterized by comprising the following steps of:
1. preparation of silicon, carbon precursor powder:
uniformly mixing polydimethylsiloxane and a curing agent, curing, then carbonizing, and adding carbonized products, phenolic resin powder and ferric nitrate powder into a high-speed mixer together for processing to obtain silicon and carbon precursor powder;
2. sintering and removing impurities:
placing the silicon and carbon precursor powder into a graphite crucible, placing the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1250-1600 ℃, reacting for 5-10 hours to obtain an initial product, and removing impurities to obtain nano silicon carbide particles based on an iron nitrate shape regulator, thereby completing the preparation method;
wherein the mass ratio of the polydimethylsiloxane to the curing agent in the first step is 9:1;
the carbonization treatment in the first step: raising the temperature to 800 ℃ at the speed of 1-3.5 ℃/min, and preserving the heat for 2-5 h;
the mass ratio of the carbonized product, the phenolic resin powder and the ferric nitrate powder in the first step is (1-50): 1;
in the second step, the temperature in the high-temperature sintering furnace is raised to 800 ℃ at a speed of 1-3.5 ℃/min, the temperature is kept for 2-5 h, then the temperature is continuously raised to 1250-1600 ℃ at a speed of 2-5 ℃/min, the temperature is kept for 5-10 h, and the cooling rate and the heating rate after the temperature is kept the same.
2. The method for preparing nano silicon carbide particles based on ferric nitrate shape regulator according to claim 1, wherein the parameters of the high-speed mixer in the step one are as follows: mixing for 5-10 h at the rotating speed of 60-100 r/min under the power of 1-20 Hz.
3. The method for preparing nano silicon carbide particles based on a ferric nitrate shape modifier according to claim 1, wherein the purity of the argon gas in the second step is 99.99%.
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