CN106219549B - The method that vacuum-sintering prepares silicon carbide nanometer line - Google Patents

The method that vacuum-sintering prepares silicon carbide nanometer line Download PDF

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CN106219549B
CN106219549B CN201610608157.1A CN201610608157A CN106219549B CN 106219549 B CN106219549 B CN 106219549B CN 201610608157 A CN201610608157 A CN 201610608157A CN 106219549 B CN106219549 B CN 106219549B
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sintering furnace
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vacuum
silicon carbide
vacuum sintering
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CN106219549A (en
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詹耀辉
胡增荣
徐家乐
郭华锋
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Suzhou University
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/22—Carbides
    • B01J27/224—Silicon carbide
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    • 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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    • C01B32/90—Carbides
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    • C01B32/956—Silicon carbide

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Abstract

The invention discloses a kind of methods that vacuum-sintering prepares silicon carbide nanometer line, comprising the following steps: step (1): first by Si and SiO2Mixing, obtains silicon class mixture, then mixes silicon class mixture with graphene, obtain mixed raw material；Step (2): mixed raw material is put into high-temperature vacuum sintering furnace, it will first be vacuumized inside high-temperature vacuum sintering furnace, then to being filled with argon gas in high-temperature vacuum sintering furnace, it will be vacuumized inside high-temperature vacuum sintering furnace again, will vacuumize, applying argon gas, vacuumize this process repetition at least 1 time again；Step (3): the mixed raw material under vacuum state in high-temperature vacuum sintering furnace is sintered, first 1400-1500 degree is heated to from room temperature in 2.5 hours, then 2 hours are kept the temperature, is finally cooled to room temperature in 2.5 hours, obtain the silicon carbide nanometer line of vacuum-sintering preparation.This method preparation efficiency is high, the silicon carbide nanometer line prepared it is linear preferably.

Description

The method that vacuum-sintering prepares silicon carbide nanometer line
Technical field
The present invention relates to silicon carbide nanometer line preparation technical fields more particularly to a kind of vacuum-sintering to prepare nanometer silicon carbide The method of line.
Background technique
With the continuous development of nanosecond science and technology, monodimension nanometer material is shown in terms of microscopic fields and nano-device development More and more important role.Such as they can be used as the needle point of scanning tunneling microscope, various sensors, microelectrode and overlarge set At the line in circuit, optical fiber, microbit and the reinforcing agent of nanocomposite etc..
Silicon carbide has a series of excellent properties, such as anti-oxidant, and resistant to chemical etching, pyroconductivity is high, and thermal stability is strong Deng, and one-dimensional silicon carbide nano material, then with physical properties such as its unique light, electrically and mechanicallies in high temperature, high frequency is powerful The electronics and optoelectronic areas of semiconductor devices and nanoscale have huge potential using value, further, since it has There are very high intensity and toughness, is but also widely used in ceramics and metal and polymeric matrix composite material.It is existing at present more The disadvantages of kind of preparation method, but the generally existing preparation efficiency of existing preparation method is low, linear difference.
In view of the above shortcomings, the designer, is actively subject to research and innovation, carbon is prepared to found a kind of vacuum-sintering The method of SiClx nano wire makes it with more the utility value in industry.
Summary of the invention
In order to solve the above technical problems, the object of the present invention is to provide the sides that a kind of vacuum-sintering prepares silicon carbide nanometer line Method, this method preparation efficiency is high, the silicon carbide nanometer line prepared it is linear preferably.
The method that a kind of vacuum-sintering proposed by the present invention prepares silicon carbide nanometer line, it is characterised in that: including following step It is rapid:
Step (1): first by Si and SiO2Mixing, obtains silicon class mixture, then mixes silicon class mixture with graphene, Obtain mixed raw material；
Step (2): mixed raw material is put into high-temperature vacuum sintering furnace, and it is true that high-temperature vacuum sintering furnace is put into high temperature In empty sintering furnace, it will first be vacuumized inside high-temperature vacuum sintering furnace, then to being filled with argon gas in high-temperature vacuum sintering furnace, then will be high Warm vacuum-sintering furnace interior vacuumizes, and will vacuumize, applying argon gas, vacuumizes this process repetition at least 1 time again；
Step (3): being sintered the mixed raw material under vacuum state in high-temperature vacuum sintering furnace, first in 2.5 hours It is heated to 1400-1500 degree from room temperature, then 2 hours is kept the temperature, is finally cooled to room temperature in 2.5 hours, obtains vacuum-sintering The silicon carbide nanometer line of preparation.
As the further improvement of the method for the present invention, Si and SiO described in step (1)2Mixed molar ratio be 0.6~ 1:1。
As the further improvement of the method for the present invention, what silicon class mixture described in step (1) was mixed with graphene rubs You are than being 1:1.5~4.
As the further improvement of the method for the present invention, the time vacuumized described in step (2) is 1 minute, is taken out Vacuum to 3Pa, the time of applying argon gas is 1 minute, applying argon gas to 1 atmospheric pressure.
As the further improvement of the method for the present invention, step vacuumizes described in (2), applying argon gas, vacuumizes this again Process is repeated 2 times.
As the further improvement of the method for the present invention, the mode heated in step (3) is from room temperature constant-speed heating to 1450 Degree, the mode of cooling are that room temperature is at the uniform velocity cooled to from 1450 degree, and the time of heating and the time of cooling are 2.5 hours.
According to the above aspect of the present invention, the present invention has at least the following advantages: the present invention is by Si, SiO2, graphene three kinds of raw materials Mixing, prepares silicon carbide nanometer line, preparation process is simple, the line for the silicon carbide nanometer line prepared in the way of vacuum-sintering Shape is preferable, due to the lamellar structure of graphene, so that it is easier to react in marginal portion with Si or SiO2, to improve system Standby efficiency, while this method can not only prepare the mixture of graphene and silicon carbide, and can directly from graphene and Pure silicon carbide is isolated in the mixture of silicon carbide.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention, And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph for the product prepared by the method for the invention in the embodiment of the present invention one；
Fig. 2 is the EDS energy spectrum diagram in the embodiment of the present invention one in scanning electron microscope (SEM) photograph box；
Fig. 3 is sintering process schematic diagram in the embodiment of the present invention one.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below Example is not intended to limit the scope of the invention for illustrating the present invention.
A kind of embodiment one: method that vacuum-sintering prepares silicon carbide nanometer line, comprising the following steps:
Step (1): first by Si and SiO20.6:1 is mixed in molar ratio, silicon class mixture is obtained, then by silicon class mixture 1:1.5 is mixed in molar ratio with graphene, obtains mixed raw material；
Step (2): mixed raw material is put into high-temperature vacuum sintering furnace, and it is true that high-temperature vacuum sintering furnace is put into high temperature In empty sintering furnace, first 3Pa will be evacuated to inside high-temperature vacuum sintering furnace, then to being filled with argon gas in high-temperature vacuum sintering furnace extremely One atmospheric pressure, then it will be evacuated to 3Pa inside high-temperature vacuum sintering furnace, it will vacuumize, applying argon gas, vacuumize this process again It is repeated 2 times, to reduce the oxygen content in high-temperature vacuum sintering furnace；
Step (3): being sintered the mixed raw material under vacuum state in high-temperature vacuum sintering furnace, first in 2.5 hours From room temperature constant-speed heating to 1450 degree, 2 hours then are kept the temperature, finally room temperature is at the uniform velocity cooled to from 1450 degree in 2.5 hours, obtains The silicon carbide nanometer line prepared to vacuum-sintering.
Electron-microscope scanning is carried out to the product of vacuum-sintering preparation, as shown in Figure 1, thread is silicon carbide nanometer line, piece Shape object is remaining graphene film.EDS power spectrum is carried out for 125 box to label in silicon carbide nanometer line electron-microscope scanning figure Analysis also just can prove that it for silicon carbide as shown in Fig. 2, illustrating that the ingredient of thread is mainly carbon and silicon.
A kind of embodiment two: method that vacuum-sintering prepares silicon carbide nanometer line, comprising the following steps:
Step (1): first by Si and SiO2In molar ratio 1:1 mix, obtain silicon class mixture, then by silicon class mixture with 1:4 is mixed graphene in molar ratio, obtains mixed raw material；
Step (2): mixed raw material is put into high-temperature vacuum sintering furnace, and it is true that high-temperature vacuum sintering furnace is put into high temperature In empty sintering furnace, first 3Pa will be evacuated to inside high-temperature vacuum sintering furnace, then to being filled with argon gas in high-temperature vacuum sintering furnace extremely One atmospheric pressure, then it will be evacuated to 3Pa inside high-temperature vacuum sintering furnace, it will vacuumize, applying argon gas, vacuumize this process again It is repeated 2 times, to reduce the oxygen content in high-temperature vacuum sintering furnace；
Step (3): being sintered the mixed raw material under vacuum state in high-temperature vacuum sintering furnace, first in 2.5 hours From room temperature constant-speed heating to 1400 degree, 2 hours then are kept the temperature, finally room temperature is at the uniform velocity cooled to from 1400 degree in 2.5 hours, obtains The silicon carbide nanometer line prepared to vacuum-sintering.
A kind of embodiment three: method that vacuum-sintering prepares silicon carbide nanometer line, comprising the following steps:
Step (1): first by Si and SiO20.6:1 is mixed in molar ratio, silicon class mixture is obtained, then by silicon class mixture 1:4 is mixed in molar ratio with graphene, obtains mixed raw material；
Step (2): mixed raw material is put into high-temperature vacuum sintering furnace, and it is true that high-temperature vacuum sintering furnace is put into high temperature In empty sintering furnace, first 3Pa will be evacuated to inside high-temperature vacuum sintering furnace, then to being filled with argon gas in high-temperature vacuum sintering furnace extremely One atmospheric pressure, then it will be evacuated to 3Pa inside high-temperature vacuum sintering furnace, it will vacuumize, applying argon gas, vacuumize this process again It is repeated 2 times, to reduce the oxygen content in high-temperature vacuum sintering furnace；
Step (3): being sintered the mixed raw material under vacuum state in high-temperature vacuum sintering furnace, first in 2.5 hours From room temperature constant-speed heating to 1500 degree, 2 hours then are kept the temperature, finally room temperature is at the uniform velocity cooled to from 1500 degree in 2.5 hours, obtains The silicon carbide nanometer line prepared to vacuum-sintering.
A kind of example IV: method that vacuum-sintering prepares silicon carbide nanometer line, comprising the following steps:
Step (1): first by Si and SiO2In molar ratio 1:1 mix, obtain silicon class mixture, then by silicon class mixture with 1:1.5 is mixed graphene in molar ratio, obtains mixed raw material；
Step (2): mixed raw material is put into high-temperature vacuum sintering furnace, and it is true that high-temperature vacuum sintering furnace is put into high temperature In empty sintering furnace, first 3Pa will be evacuated to inside high-temperature vacuum sintering furnace, then to being filled with argon gas in high-temperature vacuum sintering furnace extremely One atmospheric pressure, then it will be evacuated to 3Pa inside high-temperature vacuum sintering furnace, it will vacuumize, applying argon gas, vacuumize this process again It is repeated 2 times, to reduce the oxygen content in high-temperature vacuum sintering furnace；
Step (3): being sintered the mixed raw material under vacuum state in high-temperature vacuum sintering furnace, first in 2.5 hours From room temperature constant-speed heating to 1400 degree, 2 hours then are kept the temperature, finally room temperature is at the uniform velocity cooled to from 1400 degree in 2.5 hours, obtains The silicon carbide nanometer line prepared to vacuum-sintering.
A kind of embodiment five: method that vacuum-sintering prepares silicon carbide nanometer line, comprising the following steps:
Step (1): first by Si and SiO20.8:1 is mixed in molar ratio, silicon class mixture is obtained, then by silicon class mixture 1:3 is mixed in molar ratio with graphene, obtains mixed raw material；
Step (2): mixed raw material is put into high-temperature vacuum sintering furnace, and it is true that high-temperature vacuum sintering furnace is put into high temperature In empty sintering furnace, first 3Pa will be evacuated to inside high-temperature vacuum sintering furnace, then to being filled with argon gas in high-temperature vacuum sintering furnace extremely One atmospheric pressure, then it will be evacuated to 3Pa inside high-temperature vacuum sintering furnace, it will vacuumize, applying argon gas, vacuumize this process again It is repeated 2 times, to reduce the oxygen content in high-temperature vacuum sintering furnace；
Step (3): being sintered the mixed raw material under vacuum state in high-temperature vacuum sintering furnace, first in 2.5 hours From room temperature constant-speed heating to 1450 degree, 2 hours then are kept the temperature, finally room temperature is at the uniform velocity cooled to from 1450 degree in 2.5 hours, obtains The silicon carbide nanometer line prepared to vacuum-sintering.
The above is only a preferred embodiment of the present invention, it is not intended to restrict the invention, it is noted that for this skill For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and Modification, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (1)

1. a kind of method that vacuum-sintering prepares silicon carbide nanometer line, it is characterised in that: the following steps are included:
Step (1): first by Si and SiO2Mixing, obtains silicon class mixture, then mixes silicon class mixture with graphene, obtain Mixed raw material；
Step (2): mixed raw material is put into high-temperature vacuum sintering furnace, will first be vacuumized inside high-temperature vacuum sintering furnace, so It afterwards to being filled with argon gas in high-temperature vacuum sintering furnace, then will vacuumize, will vacuumize, applying argon gas, again inside high-temperature vacuum sintering furnace This process is vacuumized to repeat at least 1 time；
Step (3): being sintered the mixed raw material under vacuum state in high-temperature vacuum sintering furnace, first from room in 2.5 hours Temperature is heated to 1400-1500 degree, then keeps the temperature 2 hours, is finally cooled to room temperature in 2.5 hours, obtains vacuum-sintering preparation Silicon carbide nanometer line；
Si and SiO described in step (1)2Mixed molar ratio is 0.6~1:1；
The molar ratio that silicon class mixture described in step (1) is mixed with graphene is 1:1.5~4；
The time vacuumized described in step (2) is 1 minute, is evacuated to 3Pa, and the time of applying argon gas is 1 minute, is filled Argon gas is to 1 atmospheric pressure.
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PCT/CN2016/093919 WO2018018654A1 (en) 2016-07-29 2016-08-08 Method for preparing silicon carbide nanowire through vacuum sintering

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CN110872198B (en) * 2018-08-31 2022-02-15 航天特种材料及工艺技术研究所 Nanowire toughened ZrB2Preparation method of-ZrC-SiC oxidation resistant coating
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