CN112144039A - Method for preparing 3D (three-dimensional) reticular silicon carbide nanowires through nickel-carbon foam - Google Patents
Method for preparing 3D (three-dimensional) reticular silicon carbide nanowires through nickel-carbon foam Download PDFInfo
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- CN112144039A CN112144039A CN202010963657.3A CN202010963657A CN112144039A CN 112144039 A CN112144039 A CN 112144039A CN 202010963657 A CN202010963657 A CN 202010963657A CN 112144039 A CN112144039 A CN 112144039A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0209—Pretreatment of the material to be coated by heating
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention relates to a method for preparing 3D reticular silicon carbide nanowires by nickel-carbon foam, which is a simple method for preparing a 3D reticular structure containing a large amount of silicon carbide nanowires in an isothermal vertical furnace at low temperature by using a chemical vapor deposition method. The method realizes simple preparation of the 3D reticular silicon carbide nanowire, and has the advantages of low preparation temperature, good economy and wide application prospect.
Description
Technical Field
The invention belongs to a simple preparation method of a 3D reticular silicon carbide nanowire, and relates to a method for preparing the 3D reticular silicon carbide nanowire from nickel-carbon foam.
Background
The silicon carbide nano material not only has excellent comprehensive properties of high strength, high hardness, high wear resistance, oxidation resistance, high-temperature chemical stability and the like, but also has special properties of wide forbidden band, high thermal conductivity, high breakdown field strength, high electron mobility and the like, so that the silicon carbide nano material has very excellent properties in the aspects of electricity, optics and mechanics, and has wide application prospects in the fields of new energy, new materials and bioengineering. The phenomenon of burrs and the like easily occurs in the process of processing the continuous fiber reinforced ceramic matrix composite into a thin-walled part, the mechanical property of the thin-walled part is reduced, and the problem can be solved by using the one-dimensional silicon carbide nanowires to replace carbon fibers or silicon carbide fibers. The growth mechanisms of silicon carbide nanowires to date include gas-liquid-solid (VLS), gas-solid (VS). The VLS growth mechanism is mainly represented as: and (2) melting the catalyst at high temperature, dissolving gas-phase molecules in the silicon carbide nanowires into the catalyst liquid drops to form a solid solution, precipitating nuclei from the catalyst liquid drops after the dissolved silicon carbide nanowire elements are saturated, inducing the silicon carbide to grow preferentially along a certain direction by the catalyst liquid drops, and inhibiting the growth of the silicon carbide in other directions, thereby obtaining the one-dimensional nanowires. The method has the advantages of low growth temperature and easy growth of nanowires due to the induction of the catalyst. The VS method is to generate a reaction vapor source by thermal evaporation, chemical decomposition or gas phase reaction of a precursor, and condense the precursor into a one-dimensional nanomaterial on a substrate material under a certain condition after reaching a saturated state. The growth mechanism does not need a catalyst when growing the nano-wire, and the obtained target product is relatively pure, but has high requirements on production conditions. The existing preparation methods of the silicon carbide nanowires are many, but the preparation process is complex, the growth temperature is high, strict requirements on equipment and the growth process are met, and the economy is poor. In addition, the existing continuous fiber reinforced ceramic matrix composite realizes the anisotropic reinforcement of the ceramic matrix by weaving the fiber prefabricated body, and eliminates the characteristic of anisotropy, but the existing process can not weave the silicon carbide nano wire. These reasons have prevented silicon carbide nanowires from acting as the first reinforcement of the composite.
Therefore, the existing silicon carbide nanowires have complex preparation process, high temperature, strict requirements on equipment and growth process and poor economical efficiency, and cannot be woven by the existing process.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing 3D reticular silicon carbide nanowires by nickel-carbon foam, and the method is a simple method for preparing the 3D reticular silicon carbide nanowires by using a precursor at a lower temperature, and solves the problems that the yield of the silicon carbide nanowires is low, spinning and weaving cannot be performed and the like in the prior art.
Technical scheme
A method for preparing 3D reticular silicon carbide nanowires by nickel-carbon foam is characterized by comprising the following steps:
step 1: suspending the blocky nickel-carbon foam in a vertical chemical vapor deposition furnace by using a carbon rope for heat treatment, heating the chemical vapor deposition furnace to 1150-1250 ℃ at the heating rate of 6-10 ℃/min, introducing argon into a hearth at the flow rate of 300-500ml/min, preserving heat for 7h at normal pressure, and naturally cooling to obtain the nickel-carbon foam;
the volume ratio of nickel to carbon in the massive nickel-carbon foam is 6:4, and the foam structure is a 3D net shape;
step 2: suspending nickel-carbon foam in a vertical chemical vapor deposition furnace by adopting a carbon rope, electrifying to heat, heating the chemical vapor deposition furnace to 1150-1250 ℃ at the heating speed of 6-10 ℃/min, introducing argon into a hearth at the flow rate of 300-500ml/min, introducing hydrogen into the hearth at the flow rate of 1500-2500ml/min, introducing trichloromethylsilane into the hearth at the flow rate of 0.1-0.3g/min, keeping the vacuum degree at 10-20kPa, keeping the temperature for 6-8h, and then closing the program to naturally cool to obtain the 3D reticular silicon carbide nanowire deposited.
The porosity of the massive nickel carbon foam is 80-90%.
Advantageous effects
The invention provides a method for preparing 3D reticular silicon carbide nanowires by nickel-carbon foam, and provides a simple method for preparing a large amount of 3D reticular silicon carbide nanowires at a lower temperature by using one precursor through a VLS growth mechanism. The method takes trichloromethylsilane as a precursor, nickel-carbon foam as a substrate for growing the nanowire, and the 3D reticular silicon carbide nanowire grows along the reticular foam structure in the nickel-carbon foam under the catalysis of nickel element. The preparation method can realize the preparation of the 3D reticular silicon carbide nanowire, and has the advantages of simple process, low preparation temperature, good economy and wide application prospect.
The invention adopts a chemical vapor deposition process to prepare the 3D reticular silicon carbide nanowire. The silicon carbide nanowire has a series of advantages of high strength, high hardness, high oxidation resistance, high corrosion resistance, high thermal conductivity, low thermal expansion coefficient and the like, and is considered to be an ideal reinforcement for preparing a heat-insulating, high-strength and high-temperature composite material. However, the existing silicon carbide nanowires have complex preparation process, high temperature, strict requirements on equipment and growth process, poor economical efficiency, and cannot be woven by the existing process. The invention well solves the problems, and only one precursor and one catalyst are needed to prepare the 3D reticular silicon carbide nanowire.
As can be seen from the figure, a plurality of silicon carbide nanowires grow on the surface of the sample, and as can be seen from the sample pictures in figures 2-3, the prepared nanowires have uniform diameter, large length-diameter ratio and a net-shaped structure, and the main component of the nanowires is silicon carbide as can be seen from the corresponding energy spectrum pictures.
Drawings
FIG. 1: 3D reticular silicon carbide nanowire picture 7h after nickel-carbon foam deposition
FIG. 2: SEM image of 3D reticular silicon carbide nanowire deposited for 7h by nickel-carbon foam
FIG. 3: EDS spectrogram of 3D (three-dimensional) reticular silicon carbide nanowire after 7h of nickel-carbon foam deposition
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the 3D reticular silicon carbide nanowire growing method based on nickel-carbon foam comprises the following steps:
1. cutting a 60X 40X 6mm block of nickel-carbon foam (the porosity is 80-90%, wherein the volume ratio of nickel to carbon is 6:4, the foam structure is a 3D net shape), suspending the nickel-carbon foam in a vertical chemical vapor deposition furnace by using a carbon rope for heat treatment, heating the chemical vapor deposition furnace to 1150-1250 ℃ at the heating rate of 6-10 ℃/min, introducing argon into a hearth at the flow rate of 300-500ml/min, preserving heat for 7h at normal pressure, and then closing the program for naturally cooling;
2. and (2) taking the nickel-carbon foam in the step (1), suspending the nickel-carbon foam in a vertical chemical vapor deposition furnace by using a carbon rope, electrifying to heat the nickel-carbon foam, heating the chemical vapor deposition furnace to 1150-1250 ℃ at the heating speed of 6-10 ℃/min, introducing argon into the hearth at the flow rate of 300-500ml/min, introducing hydrogen into the hearth at the flow rate of 1500-2500ml/min, introducing trichloromethylsilane into the hearth at the flow rate of 0.1-0.3g/min, keeping the vacuum degree at 10-20kPa, keeping the vacuum degree at the temperature for 6-8h, and then closing the program to naturally cool to obtain the 3D reticular silicon carbide nanowire sample deposited.
The specific embodiment is as follows:
example 1
Cutting a nickel-carbon foam block sample, hanging the sample in a vertical chemical vapor deposition furnace by a carbon rope for heat treatment, heating the chemical vapor deposition furnace to 1200 ℃ at the heating rate of 7 ℃/min, introducing argon into a hearth at the flow rate of 400ml/min, and preserving heat for 7 hours at normal pressure. Suspending the nickel-carbon foam subjected to heat treatment in a constant temperature area of a vertical chemical vapor deposition furnace by using a carbon rope, heating at 7 ℃/min under the protection of Ar gas flow of 400ml/min, keeping the pressure of the furnace body to be about 10kpa, adjusting a feeding knob after heating to 1200 ℃, adjusting the feeding rate of MTS to 0.2g/min, opening H, and performing vacuum evaporation2The valve, flow rate was kept at 2500 ml/min. The deposition time is 7H, and after the deposition is finished, the electric furnace heating switch, the MTS feeding device and the H are sequentially turned off2And (4) keeping the flow of Ar at 400ml/min at an air inlet, and ensuring that the furnace chamber is cooled under vacuum. And (3) when the temperature is reduced to below 300 ℃, closing the Ar gas inlet, closing the mechanical pump, closing the cooling water, and opening the furnace body for sampling after the temperature is reduced to the room temperature, so as to obtain the 3D reticular silicon carbide nanowire sample.
Example 2
Cutting a nickel-carbon foam block sample, hanging the sample in a vertical chemical vapor deposition furnace by a carbon rope for heat treatment, heating the chemical vapor deposition furnace to 1200 ℃ at the heating rate of 7 ℃/min, introducing argon into a hearth at the flow rate of 400ml/min, and preserving heat for 7 hours at normal pressure. Heat treated nickel carbon foam with carbon ropeSuspending in constant temperature region of vertical chemical vapor deposition furnace, heating at 7 deg.C/min under protection of Ar gas flow of 400ml/min, maintaining furnace body pressure at about 15kpa, heating to 1200 deg.C, adjusting feeding knob to adjust MTS feeding rate to 0.2g/min, opening H2Valve, flow rate was maintained at 2000 ml/min. The deposition time is 7H, and after the deposition is finished, the electric furnace heating switch, the MTS feeding device and the H are sequentially turned off2And (4) keeping the flow of Ar at 400ml/min at an air inlet, and ensuring that the furnace chamber is cooled under vacuum. And (3) when the temperature is reduced to below 300 ℃, closing the Ar gas inlet, closing the mechanical pump, closing the cooling water, and opening the furnace body for sampling after the temperature is reduced to the room temperature, so as to obtain the 3D reticular silicon carbide nanowire sample.
Example 3
Cutting a nickel-carbon foam block sample, hanging the sample in a vertical chemical vapor deposition furnace by a carbon rope for heat treatment, heating the chemical vapor deposition furnace to 1230 ℃ at the heating rate of 7 ℃/min, introducing argon into a hearth at the flow rate of 400ml/min, and preserving the heat for 7 hours at normal pressure. Suspending the nickel-carbon foam subjected to heat treatment in a constant temperature area of a vertical chemical vapor deposition furnace by using a carbon rope, heating at 7 ℃/min under the protection of Ar gas flow of 400ml/min, keeping the pressure of the furnace body to be about 10kpa, adjusting a feeding knob after the temperature is increased to 1230 ℃, adjusting the feeding rate of MTS to be 0.2g/min, opening H, and performing vacuum evaporation2Valve, flow rate was maintained at 2000 ml/min. The deposition time is 7H, and after the deposition is finished, the electric furnace heating switch, the MTS feeding device and the H are sequentially turned off2And (4) keeping the flow of Ar at 400ml/min at an air inlet, and ensuring that the furnace chamber is cooled under vacuum. And (3) cooling to below 300 ℃, closing the Ar inlet, closing the mechanical pump, closing the cooling water, cooling to room temperature, opening the furnace body for sampling, and thus obtaining the 3D reticular silicon carbide nanowire sample.
In all examples, the hydrogen and argon purities were greater than 99.9%.
The invention relates to a simple method for preparing a 3D network structure containing a large amount of silicon carbide nanowires in an isothermal vertical furnace at low temperature by utilizing a chemical vapor deposition method. The method realizes simple preparation of the 3D reticular silicon carbide nanowire, and has the advantages of low preparation temperature, good economy and wide application prospect.
Claims (2)
1. A method for preparing 3D reticular silicon carbide nanowires by nickel-carbon foam is characterized by comprising the following steps:
step 1: suspending the blocky nickel-carbon foam in a vertical chemical vapor deposition furnace by using a carbon rope for heat treatment, heating the chemical vapor deposition furnace to 1150-1250 ℃ at the heating rate of 6-10 ℃/min, introducing argon into a hearth at the flow rate of 300-500ml/min, preserving heat for 7h at normal pressure, and naturally cooling to obtain the nickel-carbon foam;
the volume ratio of nickel to carbon in the massive nickel-carbon foam is 6:4, and the foam structure is a 3D net shape;
step 2: suspending nickel-carbon foam in a vertical chemical vapor deposition furnace by adopting a carbon rope, electrifying to heat, heating the chemical vapor deposition furnace to 1150-1250 ℃ at the heating speed of 6-10 ℃/min, introducing argon into a hearth at the flow rate of 300-500ml/min, introducing hydrogen into the hearth at the flow rate of 1500-2500ml/min, introducing trichloromethylsilane into the hearth at the flow rate of 0.1-0.3g/min, keeping the vacuum degree at 10-20kPa, keeping the temperature for 6-8h, and then closing the program to naturally cool to obtain the 3D reticular silicon carbide nanowire deposited.
2. The method for preparing 3D reticular silicon carbide nanowires from nickel-carbon foam according to claim 1, wherein the method comprises the following steps: the porosity of the massive nickel carbon foam is 80-90%.
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| CN202010963657.3A CN112144039A (en) | 2020-09-15 | 2020-09-15 | Method for preparing 3D (three-dimensional) reticular silicon carbide nanowires through nickel-carbon foam |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4582751A (en) * | 1984-09-04 | 1986-04-15 | Avco Corporation | Oxidation protection for carbon composite materials |
| CN105541412A (en) * | 2016-01-27 | 2016-05-04 | 南京工程学院 | Preparation method of SiC nanowire-toughened SiC ceramic coating on surface of C/C composite |
| CN108751159A (en) * | 2018-05-27 | 2018-11-06 | 南京航空航天大学 | A kind of compound carbon foam of CVI-SiC nano wires enhancing |
| CN109535644A (en) * | 2018-11-15 | 2019-03-29 | 苏州宏久航空防热材料科技有限公司 | A kind of carbon foam/carbon nanocoils/silicon carbide nanometer line resin composite materials substrate and preparation method thereof |
| CN111253159A (en) * | 2020-01-19 | 2020-06-09 | 中国科学院上海硅酸盐研究所 | Ordered and disordered SiC nanowire/whisker structure and preparation method thereof |
-
2020
- 2020-09-15 CN CN202010963657.3A patent/CN112144039A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4582751A (en) * | 1984-09-04 | 1986-04-15 | Avco Corporation | Oxidation protection for carbon composite materials |
| CN105541412A (en) * | 2016-01-27 | 2016-05-04 | 南京工程学院 | Preparation method of SiC nanowire-toughened SiC ceramic coating on surface of C/C composite |
| CN108751159A (en) * | 2018-05-27 | 2018-11-06 | 南京航空航天大学 | A kind of compound carbon foam of CVI-SiC nano wires enhancing |
| CN109535644A (en) * | 2018-11-15 | 2019-03-29 | 苏州宏久航空防热材料科技有限公司 | A kind of carbon foam/carbon nanocoils/silicon carbide nanometer line resin composite materials substrate and preparation method thereof |
| CN111253159A (en) * | 2020-01-19 | 2020-06-09 | 中国科学院上海硅酸盐研究所 | Ordered and disordered SiC nanowire/whisker structure and preparation method thereof |
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Application publication date: 20201229 |