CN111261861A - Method for continuously preparing high-purity carbon-silicon nano material - Google Patents
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention belongs to the technical field of nano materials, and relates to a method for continuously preparing a high-purity carbon-silicon nano material, which comprises the following steps: (1) inputting hydrocarbon gas and silicon-containing gas into a heating element, and carrying out thermal decomposition on the hydrocarbon gas and the silicon-containing gas in the heating element to generate carbon, silicon ions and hydrogen ions, wherein the heating element generates heat energy by adopting a plasma arc; (2) generating high-purity carbon-silicon composite or/and mixture nano material by the decomposed carbon and silicon ions in a heating element; (3) and (3) enabling the generated high-purity carbon-silicon composite or/and mixture nano material to enter a first cooling container at a high speed to obtain the stably-formed nano-sized high-purity carbon-silicon material. The method for continuously preparing the high-purity carbon-silicon nano material realizes the industrial preparation of the carbon-silicon nano material and greatly improves the purity of the carbon-silicon nano material.
Description
Technical Field
The invention belongs to the technical field of nano materials, and relates to a method for continuously preparing a high-purity carbon-silicon nano material.
Background
The conventional graphitized negative electrode material has the theoretical lithium intercalation specific capacity of 376mAh/g, and the theoretical lithium storage specific capacity of 4200mAh/g, which is 10 times as high as that of the conventional graphitized negative electrode material, but the elemental pure silicon has an expansion coefficient of more than 300% in the lithium ion intercalation process and the material itself belongs to a semiconductor material, and has poor conductivity, so that when the graphitized negative electrode material is used for the lithium ion battery negative electrode material, the defects of easy pulverization and poor rate performance of the material are caused, the elemental pure silicon is subjected to nanocrystallization and the conductivity of the material is improved, and the problem of the application of the elemental pure silicon in the lithium ion battery negative electrode material is solved.
Silicon carbide single crystals are one of the ideal third-generation semiconductors because of their unique characteristics of large forbidden bandwidth, high breakdown electric field, large thermal conductivity, high electron saturation drift velocity, small dielectric constant, strong radiation resistance, good chemical stability, etc. At present, the most effective method for growing silicon carbide crystals is a Physical Vapor Transport (PVT) method, silicon carbide powder is a main raw material for growing semiconductor silicon carbide single crystals by the PVT method, and the purity of the raw material is a key factor directly influencing the crystal quality and the electrical properties of the grown single crystals. When the nano silicon carbide is applied to a nano composite coating on the surface of a high-temperature alloy and an aviation high-performance structural ceramic, single-crystal nano silicon carbide is needed. The high-purity nano silicon carbide can also be used for preparing a nano composite coating on the surface of a high-temperature alloy, high-performance structural ceramics of an aeroengine, a wave-absorbing coating, electronic and optoelectronic devices of high-frequency, high-power, low-energy consumption, high-temperature-resistant and anti-radiation devices and the like.
The Chinese patent application CN108557823A discloses an ultra-pure nano silicon carbide and a preparation method thereof, comprising the following steps: preparing a gas reaction precursor: mixing carbon-containing gas and silicon-containing gas according to the molar ratio of Si to C of 1: 1.0-1: 1.06 to obtain a gas reaction precursor; preparing ultrapure nano silicon carbide: introducing the gas reaction precursor into the preheated ceramic reactor, and directly synthesizing the nano silicon carbide with the granularity of 50-500nm in a high-temperature region in the ceramic reactor by using the gas reaction precursor. A preparation method of ultrapure nanometer silicon carbide comprises the following steps: respectively introducing carbon-containing gas and silicon-containing gas into the preheated ceramic reactor, and mixing the carbon-containing gas and the silicon-containing gas entering the ceramic reactor according to the Si-C molar ratio of 1: 1.0-1: 1.06; the high temperature area in the ceramic reactor for carbon-containing gas and silicon-containing gas can directly synthesize nano silicon carbide with grain size of 50-500 nm. The disadvantages are that: the patent uses a ceramic container to produce silicon carbide, the pressure of the ceramic container is 1-5 atmospheric pressures, the temperature is 1100-.
The Chinese patent application CN110255532A discloses a method for macro-preparation of carbon-silicon nano-materials, which comprises the following steps: inputting hydrocarbon gas and silicon-containing gas into a plasma gun, and ionizing and thermally decomposing carbon ions, silicon ions and hydrogen ions in the plasma gun; the decomposed ions or/and silicon carbide generated by the reaction enter a cooling container, and the cooling gas released by the cooling gas ring is rapidly cooled and stably formed to generate the carbon-silicon nano material. The disadvantages are that: hydrocarbon gas and silicon-containing gas are input into a plasma gun, the hydrocarbon gas and the silicon-containing gas are ionized and thermally decomposed through a cathode region and an anode region in the plasma gun, but carbon ions and silicon ions generated by ionization decomposition can easily generate high-temperature chemical reaction with a cathode gun tip high-temperature-resistant metal alloy material in the plasma gun under the high-temperature condition to generate metal carbide and metal silicide, such as: tungsten carbide, molybdenum carbide, and metal compounds of carbon and silicon such as tungsten silicide and molybdenum silicide, etc., which pollute the purity of the carbon-silicon composite or/and mixed nanometer material or/and high-purity silicon carbide nanometer material, reduce the quality of products and have the defect of blocked application in a certain range.
Disclosure of Invention
The invention aims to provide a method for continuously preparing a high-purity carbon-silicon nano material, so that the industrial preparation of the carbon-silicon nano material is realized, and the purity of the carbon-silicon nano material is greatly improved.
The purpose of the invention is realized by the following technical means:
a method for continuously preparing high-purity carbon-silicon nano materials comprises the following steps:
(1) inputting hydrocarbon gas and silicon-containing gas into a heating element, and carrying out thermal decomposition on the hydrocarbon gas and the silicon-containing gas in the heating element to generate carbon, silicon ions and hydrogen ions, wherein the heating element generates heat energy by adopting a plasma arc;
(2) generating high-purity carbon-silicon composite or/and mixture nano material by the decomposed carbon and silicon ions in a heating element;
(3) and (3) enabling the generated high-purity carbon-silicon composite or/and mixture nano material to enter a first cooling container at a high speed to obtain a stably-formed nano-sized high-purity carbon-silicon material, wherein the temperature of the first cooling container is 50-350 ℃.
(4) Cooling the generated high-purity carbon-silicon composite or/and mixture nano material and hydrogen or chlorine-containing gas by a first cooling container, then feeding the cooled high-purity carbon-silicon composite or/and mixture nano material and hydrogen or chlorine-containing gas into a gas-solid separator, carrying out gas-solid separation, retaining the high-purity carbon-silicon composite or/and mixture nano material generated by nucleation in a bin part inside the gas-solid separator, and feeding the gas subjected to gas-solid separation into a second cooling area for continuous cooling and cyclic utilization or evacuation.
The high-purity carbon-silicon composite nano material is a carbon-silicon nano material formed by compounding carbon and silicon into the same particle, and the high-purity carbon-silicon mixed nano material is a carbon-silicon nano material formed by mixing carbon particles and silicon particles formed by carbon and silicon respectively.
The size of the nano material is 20nm-260 nm.
The temperature of the plasma arc is 5000-. The silicon-containing gas and the hydrocarbon gas enter from different temperature areas, the temperature of the area where the silicon-containing gas enters is 500-800 ℃, and the temperature of the area where the hydrocarbon gas enters is 800-1300 ℃.
The gas after gas-solid separation enters a secondary cooling area through a pipeline for cooling and recycling, and the method comprises the following steps: and the gas after gas-solid separation enters a heat exchanger for continuous cooling after passing through a pipeline, hydrogen or chlorine-containing gas is cooled to form liquid point separation, the hydrogen or/and inert gas is input into a gas storage tank, and an outlet of the gas storage tank is connected with an inner cavity of a first cooling container or a heating body channel through a pipeline and a gas flowmeter.
The heating body material is graphite or graphite with a silicon carbide coating material deposited on the surface or a high-temperature resistant metal material.
The silicon-containing gas is one or more of monosilane, dichlorosilane, trichlorosilane, silicon tetrachloride and chlorotrifluorosilane, the hydrocarbon gas is one or more of methane, ethane, acetylene, ethylene, propyne, propane and propylene, and the molar ratio of the hydrocarbon gas to the silicon-containing gas is (1-95%): (99% -5%).
The heating body comprises a feeding channel and a thermal decomposition and growth channel, the ratio of the diameter to the length of the thermal decomposition and growth channel is 1:2-200, the internal and external pressure difference of the thermal decomposition and growth channel is 0-99999pa, and the thermal decomposition and growth channel is directly communicated with the first cooling container.
The bin part in the gas-solid separator contains a discharge control valve.
Further, the generated high-purity carbon-silicon composite or/and mixed nano material is applied to a lithium ion battery cathode material or a layer of carbon material or/and conductive material is further coated on the outer surface layer of the lithium ion battery cathode material, and the high-purity carbon-silicon composite or/and mixed nano material is applied to the lithium ion battery cathode material.
The invention also provides another method for continuously preparing the high-purity carbon silicon nano material, which is used for preparing the high-purity silicon carbide nano material and comprises the following steps:
(1) inputting hydrocarbon gas and silicon-containing gas into a heating element, and carrying out thermal decomposition on the hydrocarbon gas and the silicon-containing gas in the heating element to generate carbon, silicon ions and hydrogen ions, wherein the heating element generates heat energy by adopting a plasma arc, and the temperature in the heating element is 820-;
(2) generating high-purity silicon carbide nano material by the decomposed carbon and silicon ions in the heating element;
(3) and (3) enabling the generated high-purity silicon carbide nano material to enter a first cooling container at a high speed to obtain the high-purity silicon carbide nano material with the stable forming nano size.
The prepared high-purity silicon carbide nano material is different from the prepared high-purity carbon-silicon composite or/and mixed nano material only in that: synchronously delivering the silicon-containing gas and the hydrocarbon gas to the heating element 820-1099 ℃ for synthesizing the carbon and silicon ions generated by thermal decomposition into silicon carbide. Quickly enters a first cooling container for nucleation to reach the superfine nano silicon carbide.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention compounds or/and mixes the carbon material in the pure silicon nanomaterial to improve the conductivity of the nano silicon, and synchronously cuts and separates the internal structure of the nano silicon into nano materials with carbon in the silicon and silicon in the carbon crossed vertically and horizontally, and the invention is applied to the cathode material of the lithium ion battery to greatly improve the cycle stability and rate capability of the lithium ion battery and improve the first coulombic efficiency by about 10-20%.
2. The invention adopts the hydrocarbon gas and the silicon-containing gas to directly enter the heating element which generates heat energy by the plasma arc to further carry out thermal decomposition on the gas material, greatly reduces the phenomenon that the hydrocarbon gas and the silicon-containing gas are ionized and thermally decomposed because of entering the plasma gun, the cathode high-temperature resistant alloy gun tip material and the metal material of the channel in the anode are subjected to high-temperature thermal reaction with carbon element and silicon element to consume the cathode high-temperature resistant material and the anode material, the composite or/and mixture nano material or/and silicon carbide nano material with high purity is polluted, thereby reducing the purity of the material, meanwhile, the method solves the problem that the cathode material and the anode material cannot continuously work for a long time due to consumption, greatly prolongs the continuous working time, and improves the purity of the product of the application, and the purity of the high-purity carbon silicon nano material prepared by the method can reach 99.999-99.99999%. Meanwhile, the manufacturing cost is reduced, the application range is expanded, and the additional value of the product is improved.
3. The invention adopts the heating body directly communicated with the first cooling container to prepare the carbon-silicon nano material, can discharge without stopping the machine, and further continuously prepare the carbon-silicon nano material for a long time without interruption, thereby greatly improving the production efficiency. Meanwhile, the invention adopts the pressure-free container, thereby greatly prolonging the service life of the equipment. When the silicon carbide is generated, the silicon carbide quickly enters a first cooling container, and is cooled and stably formed at the temperature of 50-350 ℃, so that the combined growth is not continued, and the size of the generated nano silicon carbide is smaller.
Detailed Description
The present invention is further illustrated by the description of the specific embodiments, but the invention is not limited thereto, and those skilled in the art can make various modifications or improvements based on the basic idea of the invention, but it is within the scope of the invention as long as they do not depart from the basic idea of the invention.
The various starting materials and reagents used in the examples of the present invention were all commercially available unless otherwise specified.
Example 1: preparation of high-purity carbon-silicon composite or/and mixture nano material
(1) The heating element of the graphite material is preheated to 500 ℃ plus 1300 ℃ and is continuously heated by a plasma arc with the temperature of 5000 ℃ plus 22000 ℃. Hydrocarbon gas such as methane and silicon-containing gas such as monosilane are mixed according to the molar ratio (1-95%): (99% -5%) are respectively fed into the heating body by means of feeding channel of heating body, and in the heating body interior the hydrocarbon-containing gas and silicon-containing gas can be undergone the process of thermal decomposition so as to produce carbon, silicon ion and hydrogen ion.
(2) The decomposed carbon and silicon ions are used for generating high-purity carbon-silicon composite or/and mixture nano-materials in the heating element.
(3) And the generated high-purity carbon-silicon composite or/and mixture nano material enters a first cooling container directly communicated with the heating body at the highest speed, and the high-purity carbon-silicon material with the stable forming nano size is obtained after cooling.
(4) And the generated high-purity carbon-silicon composite or/and mixture nano material and hydrogen or chlorine-containing gas enter a gas-solid separator for gas-solid separation, the nucleated high-purity carbon-silicon composite or/and mixture nano material is retained in a bin part in the gas-solid separator, and the bin part is provided with a discharge valve for timed discharge to form continuous discharge without stopping.
(5) The gas separated by gas-solid enters a heat exchanger for continuous cooling after passing through a pipeline, hydrogen or chlorine-containing gas is cooled to form liquid point separation, the hydrogen or/and inert gas is input into a gas storage tank, and an outlet of the gas storage tank is connected with an inner cavity of a first cooling container or a heating body channel through a pipeline and a gas flowmeter.
(6) The generated high-purity carbon-silicon composite or/and mixed nano material is applied to a lithium ion battery cathode material or a layer of carbon material or/and conductive material is further coated on the outer surface layer of the lithium ion battery cathode material, and the high-purity carbon-silicon composite or/and mixed nano material is applied to the lithium ion battery cathode material.
Example 2: preparation of high purity silicon carbide nano material
(1) The method comprises the steps of preheating a heating body made of graphite materials with a high-temperature region and a low-temperature region to 820-.
(2) And generating the high-purity silicon carbide nano material by the decomposed carbon and silicon ions in the heating element.
(3) The generated high-purity silicon carbide nano material enters a first cooling container directly communicated with the heating body at the highest speed, and the high-purity silicon carbide material with the stable forming nano size is obtained after cooling.
(4) And the generated high-purity silicon carbide nano material and hydrogen or chlorine-containing gas enter a gas-solid separator for gas-solid separation, the nucleated high-purity silicon carbide nano material is retained in a bin part in the gas-solid separator, and the bin part is provided with a discharge valve for timed discharge to form continuous discharge without stopping.
(5) The gas separated by gas-solid enters a heat exchanger for continuous cooling after passing through a pipeline, hydrogen or chlorine-containing gas is cooled to form liquid point separation, the hydrogen or/and inert gas is input into a gas storage tank, and an outlet of the gas storage tank is connected with an inner cavity of a first cooling container or a heating body channel through a pipeline and a gas flowmeter.
(6) The generated high-purity silicon carbide nano material is applied to a silicon carbide crystal growth raw material.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (10)
1. A method for continuously preparing high-purity carbon-silicon nano materials is characterized by comprising the following steps:
(1) inputting hydrocarbon gas and silicon-containing gas into a heating element, and carrying out thermal decomposition on the hydrocarbon gas and the silicon-containing gas in the heating element to generate carbon, silicon ions and hydrogen ions, wherein the heating element generates heat energy by adopting a plasma arc;
(2) generating high-purity carbon-silicon composite or/and mixture nano material by the decomposed carbon and silicon ions in a heating element;
(3) and (3) enabling the generated high-purity carbon-silicon composite or/and mixture nano material to enter a first cooling container at a high speed to obtain the stably-formed nano-sized high-purity carbon-silicon material.
2. The method of claim 1, wherein the steps further comprise:
(4) cooling the generated high-purity carbon-silicon composite or/and mixture nano material and hydrogen or chlorine-containing gas by a first cooling container, then feeding the cooled high-purity carbon-silicon composite or/and mixture nano material and hydrogen or chlorine-containing gas into a gas-solid separator, carrying out gas-solid separation, retaining the high-purity carbon-silicon composite or/and mixture nano material generated by nucleation in a bin part inside the gas-solid separator, and feeding the gas subjected to gas-solid separation into a second cooling area for continuous cooling and cyclic utilization or evacuation.
3. The method for continuously preparing high-purity carbon-silicon nanomaterial according to claim 2, wherein the gas after gas-solid separation enters the second cooling region through a pipeline and is cooled and recycled in a way that: and the gas after gas-solid separation enters a heat exchanger for continuous cooling after passing through a pipeline, hydrogen or chlorine-containing gas is cooled to form liquid point separation, the hydrogen or/and inert gas is input into a gas storage tank, and an outlet of the gas storage tank is connected with an inner cavity of a first cooling container or a heating body channel through a pipeline and a gas flowmeter.
4. The method as claimed in claim 1, wherein the temperature of the plasma arc is 5000-.
5. The method for continuously preparing the high-purity carbon silicon nanomaterial as claimed in claim 1, wherein the heating element material is graphite or graphite with a silicon carbide coating material deposited on the surface or a high-temperature resistant metal material.
6. The method as claimed in claim 1, wherein the silicon-containing gas is one or more of monosilane, dichlorosilane, trichlorosilane, silicon tetrachloride and chlorotrifluorosilane, the hydrocarbon gas is one or more of methane, ethane, acetylene, ethylene, propyne, propane and propylene, and the molar ratio of the hydrocarbon gas to the silicon-containing gas is (1% -95%): (99% -5%).
7. The method of claim 1, wherein the heating element comprises a feeding channel and a thermal decomposition and growth channel, the ratio of the diameter to the length of the thermal decomposition and growth channel is 1:2-200, the pressure difference between the inside and the outside of the thermal decomposition and growth channel is 0-99999pa, and the thermal decomposition and growth channel is directly communicated with the first cooling container.
8. The method for continuously preparing the high-purity carbon-silicon nanomaterial according to any one of claims 1 to 7, wherein the generated high-purity carbon-silicon composite or/and mixed nanomaterial is applied to a negative electrode material of a lithium ion battery or is further coated with a layer of carbon material or/and conductive material on the outer surface layer of the negative electrode material of the lithium ion battery.
9. A method for continuously preparing high-purity carbon-silicon nano materials is characterized by comprising the following steps:
(1) inputting hydrocarbon gas and silicon-containing gas into a heating element, and carrying out thermal decomposition on the hydrocarbon gas and the silicon-containing gas in the heating element to generate carbon, silicon ions and hydrogen ions, wherein the heating element generates heat energy by adopting a plasma arc, and the temperature in the heating element is 820-;
(2) generating high-purity silicon carbide nano material by the decomposed carbon and silicon ions in the heating element;
(3) and (3) enabling the generated high-purity silicon carbide nano material to enter a first cooling container at a high speed to obtain the high-purity silicon carbide nano material with a stable forming nano size.
10. The method of claim 9, wherein the silicon-containing gas is monosilane, and the hydrocarbon gas is methane.
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| CN113072039A (en) * | 2021-03-29 | 2021-07-06 | 浙江中宁硅业有限公司 | Method for preparing silicon-carbon composite material by using silane tail gas |
| CN114225852A (en) * | 2021-12-17 | 2022-03-25 | 浙江中宁硅业有限公司 | Method and device for preparing silicon-carbon composite material based on gas phase decomposition method |
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