CN111484017A - Method for preparing SiC nanoparticles based on silica microspheres @ C - Google Patents
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- CN111484017A CN111484017A CN202010573895.3A CN202010573895A CN111484017A CN 111484017 A CN111484017 A CN 111484017A CN 202010573895 A CN202010573895 A CN 202010573895A CN 111484017 A CN111484017 A CN 111484017A
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- 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
- C01B32/97—Preparation from SiO or SiO2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- 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
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- 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
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
A method for preparing SiC nano-particles based on silicon dioxide microspheres @ C belongs to the technical field of silicon carbide preparation and ceramic powder material preparation, and aims to solve the problems of complex process, low purity and uneven particle size distribution existing in the existing preparation of silicon carbide nano-powder. The method comprises the following steps: firstly, preparing SiO2@ phenolic resin precursor powder; II, preparing SiO2@ C powder; III, SiO2Cooling the microspheres @ C powder to room temperature after high-temperature sintering to obtain the SiO-based powder2And preparing SiC nano particles by using the microspheres @ C. The invention takes phenolic resin as a carbon source, and after high-temperature carbonization reaction, the phenolic resin is in SiO2The surface is uniformly coated with a layer of carbon and SiO2As a silicon source and a morphology template, under the catalysis of copper nitrate, the nano-scale silicon carbide powder with uniform particle size distribution is successfully prepared by the carbothermic reduction reaction. The preparation method is simple, the product purity is high, and the particle size distribution is uniform. The method is applied to the preparation of the nano silicon carbide particles.
Description
Technical Field
The invention belongs to the technical field of silicon carbide preparation and ceramic powder material preparation, and particularly relates to a preparation method of SiC nano particles.
Background
The SiC crystal has strong ionic covalent bond and high Si-C bond energy, so that the SiC material has high modulus, high strength and high hardness. The SiC has stable chemical property, strong acid resistance and strong alkali resistance and has better performanceCan form SiO on the SiC surface in a high-temperature oxidizing atmosphere2The layer prevents further oxidation. The SiC material also has excellent high-temperature stability and radiation resistance, and is a structural material with high comprehensive performance. Meanwhile, SiC is a wide bandgap semiconductor, has the characteristics of high thermal conductivity, large electronic saturation mobility and high critical breakdown voltage, is suitable for being used in extreme environments such as high temperature, high radiation and the like, and therefore has wide application value in the field of semiconductors. Silicon carbide can exert mechanical bearing performance in important equipment, and sintering activity plays an important influence role in the mechanical performance of the final ceramic product. In the industry, the pressureless sintered silicon carbide powder can be made into ceramic sealing rings, the global market total of the silicon carbide sealing rings reaches 20 hundred million dollars, but the sealing rings in China are in middle and low-grade markets, and the silicon carbide sealing ring market with high end and high profit is monopolized by Germany. The reason for this is that the density of the silicon carbide sealing ring in China is only 3.10, holes exist in the sealing ring, and the service life of the sealing ring is extremely short under the working conditions of high load and rapid rotation. The density of the silicon carbide sealing ring produced by Germany can reach 3.16, the ceramic structure is almost completely compact, and the high-speed rotation of dozens of thousands of times under the working conditions of high load and quick rotation is met. In the aspect of national defense application, silicon carbide is a very important electromagnetic wave absorbing material, and compared with wave absorbing materials such as carbonyl iron, carbon nano tubes and graphene, the silicon carbide has very high chemical stability, does not generate galvanic corrosion in the actual use process, is dispersed in resin or ceramic matrix, can exert the effect of mechanical toughening, can be used in severe environments such as sea surface and high temperature, and is a strategic key material in China. The prior preparation technology of the silicon carbide powder has the defects of high cost, high reaction temperature, difficult process control, complex process, low yield, lower purity of the synthesized powder, uneven particle size distribution of powder particles, easy agglomeration of the powder particles and the like. Therefore, by researching the thermodynamic nucleation and the kinetic growth behavior of the nano silicon carbide powder, the technology of controllable growth 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 complex process, low purity and uneven particle size distribution of the existing preparation of silicon carbide nano powder, and provides a method for preparing SiC nano particles based on silicon dioxide microspheres @ C.
A method for preparing SiC nano-particles based on silica microspheres @ C comprises the following steps:
SiO 22Preparation of @ phenolic resin precursor powder:
dissolving phenolic resin in 20-30% ethanol solution to form binder solution, and adding SiO2Mechanically stirring the microspheres for 1 to 4 hours at the temperature of between 40 and 60 ℃ at the rotating speed of 1200 to 1500r/min to obtain SiO2Injecting the microsphere/phenolic resin dispersion into the catalyst solution for aging of the phenolic resin and loading of the catalyst, and drying to obtain SiO2@ phenolic resin precursor powder;
II, SiO2Preparation of @ C powder:
SiO obtained in the step one2The precursor powder of the @ phenolic resin is carbonized under inert gas to obtain SiO2Microsphere @ C powder;
thirdly, the SiO obtained in the second step2Putting the microspheres @ C powder into a graphite crucible, putting the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1300-1800 ℃, reacting for 1-6 h, and cooling to room temperature to finish the SiO-based reaction2Preparing SiC nanoparticles by using the microspheres @ C;
wherein the catalyst solution in the first step is a copper nitrate solution with the mass fraction of 1-3%.
The principle and the beneficial effects of the invention are as follows:
the method adopts copper nitrate as a catalyst, plays the role of Cu ions, and promotes the in-situ solid-phase reaction of a carbon source and a silicon source to generate silicon carbide, thereby controlling the growth of the grain size.
The invention takes phenolic resin as a carbon source, and after high-temperature carbonization reaction, the phenolic resin is in SiO2The surface is uniformly coated with a layer of carbon and SiO2As a silicon source and a shape template inPromoting the generation of in-situ solid phase reaction generated by the silicon carbide particles under the catalysis of the copper nitrate, and successfully preparing the nano silicon carbide powder with uniform particle size distribution through the carbothermic reduction reaction. The preparation method is simple, the product has high purity and uniform particle size distribution, and is suitable for large-scale industrial production.
The method is applied to the preparation of the nano silicon carbide particles.
Drawings
FIG. 1 is an XRD spectrum of SiC nanoparticles prepared in example;
fig. 2 is a microscopic morphology of the SiC nanoparticles 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 embodiment of the invention relates to a method for preparing SiC nano particles based on silica microspheres @ C, which is realized by the following steps:
SiO 22Preparation of @ phenolic resin precursor powder:
dissolving phenolic resin in 20-30% ethanol solution to form binder solution, and adding SiO2Mechanically stirring the microspheres for 1 to 4 hours at the temperature of between 40 and 60 ℃ at the rotating speed of 1200 to 1500r/min to obtain SiO2Injecting the microsphere/phenolic resin dispersion into the catalyst solution for aging of the phenolic resin and loading of the catalyst, and drying to obtain SiO2@ phenolic resin precursor powder;
II, SiO2Preparation of @ C powder:
SiO obtained in the step one2The precursor powder of the @ phenolic resin is carbonized under inert gas to obtain SiO2Microsphere @ C powder;
fourthly, SiO obtained in the second step2Putting the microspheres @ C powder into a graphite crucible, putting the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1300-1800 ℃, reacting for 1-6 h, and cooling to room temperature to finish the SiO-based reaction2Preparing SiC nanoparticles by using the microspheres @ C;
wherein the catalyst solution in the first step is a copper nitrate solution with the mass fraction of 1-3%.
The phenolic resin in step one of the present embodiment serves as a carbon source.
SiO in step one of the present embodiment2The microspheres are used as silicon source.
In the first step of the embodiment, the drying is performed at 80 ℃ for 30-50 min.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that the volume ratio of the phenolic resin to the ethanol solution with the mass concentration of 20-30% in the first embodiment is 1 (2-4). Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: the difference between the present embodiment and the first or second embodiment is that the SiO in the first step2The particle size of the microspheres is 10-30 nm. Other steps and parameters are the same as those in the first or second embodiment.
The fourth concrete implementation mode: this embodiment differs from one of the first to third embodiments in that the aging of the phenol resin and the loading of the catalyst in the first step: stirring for 1-4 h at 40-60 ℃ in a water bath. Other steps and parameters are the same as those in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is that the SiO in the first step2The volume ratio of the microsphere/phenolic resin dispersion liquid to the deionized water is 1 (1-5). Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is that in the first step, the mixture is mechanically stirred at a rotation speed of 1400r/min for 2h at 50 ℃. Other steps and parameters are the same as those in one of the first to fifth embodiments.
The seventh embodiment: this embodiment differs from the first to sixth embodiments in that the carbonization treatment is performed under an inert gas in the second step: SiO 22@ phenolic resin precursor powder was placed in a programmable quartz tube furnace and flowedHeating to 700-900 ℃ in Ar atmosphere, and keeping the temperature for 2-4 h. Other steps and parameters are the same as those in one of the first to sixth embodiments.
The specific implementation mode is eight: the seventh embodiment is different from the seventh embodiment in that the purity of the Ar gas is 99.9%. Other steps and parameters are the same as those in the seventh embodiment.
The specific implementation method nine: seventh or eighth embodiment is different from the seventh or eighth embodiment in that the rate of temperature rise is 0.5 to 2 ℃/min. Other steps and parameters are the same as those of the seventh or eighth embodiment.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is that the temperature is raised to 1750 ℃ in the third step and the reaction is carried out for 3 hours. Other steps and parameters are the same as those in one of the first to ninth embodiments.
The concrete implementation mode eleven: the present embodiment is different from the first to tenth embodiments in that the temperature rise in the third step is: heating to 1000 ℃ at the speed of 5-10 ℃/min, and then continuously heating to 1300-1800 ℃ at the speed of 2.5-5 ℃/min. Other steps and parameters are the same as in one of the first to tenth embodiments.
The specific implementation mode twelve: this embodiment differs from one of the first to eleventh embodiments in that the cooling in step three is: cooling to room temperature at a rate of 5-10 ℃/min. Other steps and parameters are the same as those in one of the first to eleventh embodiments.
The beneficial effects of the present invention are demonstrated by the following examples:
example (b):
a method for preparing SiC nano-particles based on silica microspheres @ C comprises the following steps:
SiO 22Preparation of @ phenolic resin precursor powder:
dissolving phenolic resin in 30% ethanol solution to form binder solution, and adding SiO2Mechanically stirring the microspheres for 2 hours at the temperature of 45 ℃ at the rotating speed of 1500r/min to obtain SiO2Injecting the microsphere/phenolic resin dispersion into the copper nitrate solutionAging phenolic resin and loading catalyst, drying to obtain SiO2@ phenolic resin precursor powder;
II, SiO2Preparation of @ C powder:
SiO obtained in the step one2The precursor powder of the @ phenolic resin is carbonized under inert gas to obtain SiO2Microsphere @ C powder;
thirdly, the SiO obtained in the second step2Putting the microspheres @ C powder into a graphite crucible, putting the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1700 ℃ for reaction for 2 hours, and then cooling to room temperature to finish the SiO-based reaction2Preparing SiC nanoparticles by using the microspheres @ C;
wherein the catalyst solution in the first step is a copper nitrate solution with the mass fraction of 2%.
In the first step of this example, the volume ratio of the phenolic resin to the 30% ethanol solution is 1: 2.
In the first step of this embodiment, the SiO2The particle size of the microspheres is 20 nm.
The aging of the phenolic resin and the loading of the catalyst in the first step of this example: the mixture was stirred for 2h while heating in a water bath at 45 ℃.
In the first step of this embodiment, the SiO2The volume ratio of the microsphere/phenolic resin dispersion to the deionized water was 1: 2.
In the second step of this example, the carbonization treatment was performed under an inert gas: SiO 22The @ phenolic resin precursor powder is placed in a programmable quartz tube furnace, the temperature is raised to 800 ℃ under the flowing Ar atmosphere, and the heat preservation time is 3 hours; the purity of the Ar gas is 99.9 percent; the rate of temperature rise is 0.5 ℃/min.
In the third step of this embodiment, the temperature rise is: the temperature is raised to 1000 ℃ at the rate of 5 ℃/min, and then the temperature is raised to 1700 ℃ at the rate of 3 ℃/min.
The cooling in step three of this example is: the temperature is reduced to room temperature at a rate of 5 ℃/min.
In the embodiment, phenolic resin is used as a carbon source, and after high-temperature carbonization reaction, the phenolic resin is on SiO2The surface is uniformly coated with a layer of carbon and SiO2As a silicon source and a morphology template, the nanometer silicon carbide powder with uniform particle size distribution is successfully prepared through a carbothermic reduction reaction.
The X-ray diffraction (XRD) spectrum of the SiC nanoparticles 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, and no impurity peak is found, which indicates that β -SiC material can be successfully prepared by the method of this example, and the product purity is high.
The microscopic morphology of the SiC nanoparticles prepared in this example; as can be seen from FIG. 2, SiO is used2The surface of the microsphere is coated with phenolic resin, and the in-situ solid phase reaction generated by the silicon carbide particles is promoted under the catalysis of copper nitrate, so that the silicon carbide particles with uniform particle size distribution and average size of 35.5 nanometers are successfully prepared.
Claims (10)
1. A method for preparing SiC nano-particles based on silica microspheres @ C is characterized by comprising the following steps:
SiO 22Preparation of @ phenolic resin precursor powder:
dissolving phenolic resin in 20-30% ethanol solution to form binder solution, and adding SiO2Mechanically stirring the microspheres for 1 to 4 hours at the temperature of between 40 and 60 ℃ at the rotating speed of 1200 to 1500r/min to obtain SiO2Injecting the microsphere/phenolic resin dispersion into the catalyst solution for aging of the phenolic resin and loading of the catalyst, and drying to obtain SiO2@ phenolic resin precursor powder;
II, SiO2Preparation of @ C powder:
SiO obtained in the step one2The precursor powder of the @ phenolic resin is carbonized under inert gas to obtain SiO2Microsphere @ C powder;
thirdly, the SiO obtained in the second step2Putting the microspheres @ C powder into a graphite crucible, putting the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1300-1800 ℃, reacting for 1-6 h, and cooling to room temperature to finish the SiO-based reaction2Preparing SiC nanoparticles by using the microspheres @ C;
wherein the catalyst solution in the first step is a copper nitrate solution with the mass fraction of 1-3%.
2. The method for preparing SiC nanoparticles based on silica microspheres @ C as claimed in claim 1, wherein the volume ratio of the phenolic resin to the ethanol solution with the mass concentration of 20-30% in the step one is 1 (2-4).
3. The method for preparing SiC nano-particles based on silica microspheres @ C as claimed in claim 1, wherein the SiO in step one2The particle size of the microspheres is 10-30 nm.
4. The method for preparing SiC nano-particles based on silica microspheres @ C as claimed in claim 1, wherein the aging of the phenolic resin and the loading of the catalyst in the step one: stirring for 1-4 h at 40-60 ℃ in a water bath.
5. The method for preparing SiC nano-particles based on silica microspheres @ C as claimed in claim 1, wherein the SiO in step one2The volume ratio of the microsphere/phenolic resin dispersion liquid to the deionized water is 1 (1-5).
6. The method for preparing SiC nano-particles based on silica microspheres @ C as claimed in claim 1, wherein the carbonization treatment is performed under inert gas in the second step: SiO 22The @ phenolic resin precursor powder is placed in a programmable quartz tube furnace, the temperature is raised to 700-900 ℃ under the flowing Ar atmosphere, and the heat preservation time is 2-4 h.
7. The method for preparing SiC nanoparticles based on silica microspheres @ C as claimed in claim 6, wherein the rate of temperature rise is 0.5-2 ℃/min.
8. The method for preparing SiC nano-particles based on silica microspheres @ C as claimed in claim 1, wherein in step three, the temperature is raised to 1750 ℃ for reaction for 3 h.
9. The method for preparing SiC nanoparticles based on silica microspheres @ C as claimed in claim 1, wherein the temperature rise in step three is: heating to 1000 ℃ at the speed of 5-10 ℃/min, and then continuously heating to 1300-1800 ℃ at the speed of 2.5-5 ℃/min.
10. The method for preparing SiC nano-particles based on silica microspheres @ C as claimed in claim 1, wherein the cooling in step three is: cooling to room temperature at a rate of 5-10 ℃/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114261966A (en) * | 2021-12-13 | 2022-04-01 | 江西省矿产资源保障服务中心 | Method for synthesizing submicron silicon carbide spheres by using carbon-containing silicon dioxide powder with low energy consumption |
| CN114956044A (en) * | 2022-07-12 | 2022-08-30 | 国环电池科技(苏州)有限公司 | Method for quickly and efficiently preparing hollow carbon microspheres |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1946655A (en) * | 2004-04-23 | 2007-04-11 | 丰田自动车株式会社 | Composite carbon material having metal carbide particles dispersed therein and method for preparation thereof |
| CN101774813A (en) * | 2010-01-20 | 2010-07-14 | 中国科学院山西煤炭化学研究所 | Method for preparing small-sized silicon carbide or silicon nitride nano particles from waste plastics |
| CN101804981A (en) * | 2010-04-01 | 2010-08-18 | 中国科学院山西煤炭化学研究所 | Method for preparing hollow silicon carbide nano material |
| CN102295286A (en) * | 2011-06-16 | 2011-12-28 | 北京化工大学 | Preparation method of beta-silicon carbide nano-fiber by Fe catalysis |
| CN103553043A (en) * | 2013-09-30 | 2014-02-05 | 陕西科技大学 | Preparation method for SiC nanometer microsphere with high specific surface area |
| CN104844225A (en) * | 2015-06-08 | 2015-08-19 | 齐鲁工业大学 | SiC-coated hexagonal boron nitride composite powder modified self-lubricating ceramic cutter material and preparation method thereof |
| CN105692622A (en) * | 2016-03-18 | 2016-06-22 | 宁夏大学 | Preparation method of nanoscale silicon carbide particles and product of nanoscale silicon carbide particles |
| CN108598395A (en) * | 2018-03-30 | 2018-09-28 | 武汉理工大学 | The magnanimity preparation method of monodisperse silica/nitrogen-doped carbon composite Nano ball or microballoon |
| CN109748282A (en) * | 2019-03-25 | 2019-05-14 | 东北大学 | A kind of method of low temperature preparation nanometer silicon carbide |
| CN110819302A (en) * | 2019-11-07 | 2020-02-21 | 哈尔滨工业大学 | Preparation method of silicon carbide/carbon hollow porous microsphere wave-absorbing material |
-
2020
- 2020-06-22 CN CN202010573895.3A patent/CN111484017A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1946655A (en) * | 2004-04-23 | 2007-04-11 | 丰田自动车株式会社 | Composite carbon material having metal carbide particles dispersed therein and method for preparation thereof |
| CN101774813A (en) * | 2010-01-20 | 2010-07-14 | 中国科学院山西煤炭化学研究所 | Method for preparing small-sized silicon carbide or silicon nitride nano particles from waste plastics |
| CN101804981A (en) * | 2010-04-01 | 2010-08-18 | 中国科学院山西煤炭化学研究所 | Method for preparing hollow silicon carbide nano material |
| CN102295286A (en) * | 2011-06-16 | 2011-12-28 | 北京化工大学 | Preparation method of beta-silicon carbide nano-fiber by Fe catalysis |
| CN103553043A (en) * | 2013-09-30 | 2014-02-05 | 陕西科技大学 | Preparation method for SiC nanometer microsphere with high specific surface area |
| CN104844225A (en) * | 2015-06-08 | 2015-08-19 | 齐鲁工业大学 | SiC-coated hexagonal boron nitride composite powder modified self-lubricating ceramic cutter material and preparation method thereof |
| CN105692622A (en) * | 2016-03-18 | 2016-06-22 | 宁夏大学 | Preparation method of nanoscale silicon carbide particles and product of nanoscale silicon carbide particles |
| CN108598395A (en) * | 2018-03-30 | 2018-09-28 | 武汉理工大学 | The magnanimity preparation method of monodisperse silica/nitrogen-doped carbon composite Nano ball or microballoon |
| CN109748282A (en) * | 2019-03-25 | 2019-05-14 | 东北大学 | A kind of method of low temperature preparation nanometer silicon carbide |
| CN110819302A (en) * | 2019-11-07 | 2020-02-21 | 哈尔滨工业大学 | Preparation method of silicon carbide/carbon hollow porous microsphere wave-absorbing material |
Non-Patent Citations (3)
| Title |
|---|
| 张建强等: "中空碳化硅微球的制备及其在催化NaBH4制氢中的应用", 《华东理工大学学报（自然科学版）》 * |
| 王军凯等: "Fe催化硅藻土碳热还原反应制备3C-SiC及其机理", 《材料研究学报》 * |
| 赵春荣等: "核壳结构SiC/SiO2纳米线的低温合成与表征", 《无机材料学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114261966A (en) * | 2021-12-13 | 2022-04-01 | 江西省矿产资源保障服务中心 | Method for synthesizing submicron silicon carbide spheres by using carbon-containing silicon dioxide powder with low energy consumption |
| CN114261966B (en) * | 2021-12-13 | 2024-01-30 | 江西省矿产资源保障服务中心 | Method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption |
| CN114956044A (en) * | 2022-07-12 | 2022-08-30 | 国环电池科技(苏州)有限公司 | Method for quickly and efficiently preparing hollow carbon microspheres |
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Application publication date: 20200804 |