CN107200331A - A kind of preparation method of open system SiC nanowire - Google Patents
A kind of preparation method of open system SiC nanowire Download PDFInfo
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- CN107200331A CN107200331A CN201710550930.8A CN201710550930A CN107200331A CN 107200331 A CN107200331 A CN 107200331A CN 201710550930 A CN201710550930 A CN 201710550930A CN 107200331 A CN107200331 A CN 107200331A
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Abstract
The invention discloses a kind of preparation method of open system SiC nanowire.The silica crucible for filling metallic silicon power is put into tube furnace intermediate region, and graphite paper is laid in the low-temperature zone of tube furnace；Temperature according to required for reaction sets the heating schedule of tube furnace, and reaction soaking time is set according to the number of liquid carbon source injection volume；When the temperature required for temperature reaches reaction, the digital injection pump of liquid carbon source is opened, carbon source is injected in tube furnace, liquid carbon source obtains carbon source by Pintsch process gasification, then tube furnace conversion zone is delivered to by argon gas and carry out carbothermic reduction reaction；After liquid carbon source injection terminates, start startup cooling process and be down to normal temperature, deposition has SiC nanowire on graphite paper.The present invention uses ethanol or propyl alcohol for carbon source first, and silica flour is silicon source, and SiC nanowire is prepared in open system.Compared to background technology, with low energy expenditure, technique is simple, the advantages of preparing without catalyst and continuously.
Description
Technical field
The present invention relates to a kind of preparation method of SiC nanowire, a kind of open system SiC nanowire is particularly related to
Preparation method.
Background technology
In the research of numerous monodimension nanometer materials, the synthesis transitivity of wide band gap semiconducter one-dimensional material, which studies oneself, to be turned into
One of main study hotspot.And in these wide bandgap semiconductor materials, SiC crystal material is a kind of direct wide band gap semiconducter
Material, its normal temperature energy gap is 3.0eV, with the characteristic such as high saturated electrons drift speed and electric conductivity, as make high frequency,
The ideal material of high-power, low energy consumption, high temperature resistant and radioresistance device.
Monodimension nanometer material has more superior performance compared to body material.One-dimensional carbofrax material is imitated due to quantum size
Should, small-size effect and skin effect, with more excellent luminescent properties, electric property, Field emission property and photocatalytic effect.
In addition, carborundum monodimension nanometer material is in probe and sensing and enhancing composite of hydrogen storage and AFM etc.
Field is all widely used.
In view of the excellent properties of one-dimensional carbofrax material, researcher has done substantial amounts of with regard to the preparation of silicon carbide nanometer line
Work.J.J.Niu, J.N. Wang are in 2007 in European Journal of Inorganic Chemistry（Europe
Inorganic chemistry magazine, 2007,4006~4010）Deliver entitled：An Approach to the Synthesis of
Silicon Carbide Nanowires by Simple Thermal Evaporation of Ferrocene onto
Silicon Wafers（Ferrocene thermal evaporation synthesizing silicon carbide nano wire on silicon wafer surface）Article.By silicon wafer in text
Pyroreaction section is placed on, and lays ferrocene powder on silicon, when temperature reaches 1550 DEG C, ferrocene pyrolysis produces carbon
With catalyst iron with this synthesizing silicon carbide nano wire.In the method, ferrocene before reaction temperature is reached will because of vaporization at high temperature,
And it can only be contacted with silicon chip surface, the nano wire yield of gained is less.
J.Zhu etc. is reported with SiCl4For silicon source, C6H6For carbon source, ferrocene is catalyst in SiCl4-C6H6-H2- Ar
Synthetizing silicon carbide nano rods under system（Solid State Communications, 118 (2001), 595-598）, the method
Equipment sets complex, and C6H6It is poisonous, have a strong impact on the healthy of operating personnel.
ZL201410675593.1 discloses a kind of method for preparing silicon carbide nanometer line, by organic phenolic resin and inorganic
Silica flour mechanical mixture, is fitted into porcelain Noah's ark, is incubated 1~4h at 1200 DEG C~1400 DEG C under argon gas protection, is then cooled back to
Normal temperature, you can obtain the nano wire of carborundum.
ZL 201410653437.5 discloses a kind of method for preparing silicon carbide nanometer line, according to carbon and element silicon
Mol ratio be (3~1):1 weighs graphite, silicon and silica, and wherein silicon is identical with the amount of the material of silica；Claim again
Take catalyst, the mass ratio of catalyst and silicon is (5~20%):1, all raw materials are mixed, 8~30h of ball milling are carried out, then
Porcelain Noah's ark is put into after drying and is pushed into tube furnace center, under argon gas protection, condition of normal pressure, 1150~1350 DEG C, reaction 1 is warming up to
~4h, then be down to normal temperature, that is, obtain ultra-long silicon carbide nano-wires.
ZL 200610049667.6 discloses a kind of method of synthetizing silicon carbide nano rods, is that broken silicon wafers are placed in into graphite
In crucible, the porous oxidation aluminium substrate for filling CNT is positioned on crucible, another black-fead crucible is then inverted in substrate
On；By crucible place vacuum high-temperature sintering stove in, with 10~30 DEG C/min heating rate be warming up to always 1400 DEG C~
1600 DEG C, 3~6 hours of soaking time, silicon vapor is reacted with CNT, and whole device is carried out under the atmosphere of argon gas, instead
After should terminating, turn off heating power supply, cool down；Finally there is substantial amounts of linen nano SiC rod powder product to be attached to substrate
On.
In summary, the preparation of silicon carbide nanometer line is typically to be carried out in the reaction system of closing.Do not exist still at present
In open system, and the precedent of silicon carbide nanometer line is prepared using ethanol or propyl alcohol as carbon source.Prepare nanometer silicon carbide at present
General line is mainly silicon source using silica flour, silica or silicon tetrachloride in closed system, and graphite flake, phenolic resin are
Carbon source or organic cracking carbon obtain carbon source.These methods easily produce the impurity either solid matter of other catabolites
Residual, nano wire purity and uniformity obtained by preparing can influence, and yield is nor very high, in the space of closing
Also the continuous preparation of silicon carbide nanometer line can not be realized.
The content of the invention
In order to overcome problem present in background technology field, received it is an object of the invention to provide a kind of open system SiC
The preparation method of rice noodles, is that a kind of method is simple, low energy expenditure cost, and workable, can carry out large-scale industry
Production, first using silica flour as silicon source in open system, carbon source is obtained by Pintsch process using ethanol as carbon source, in inertia
The method for obtaining SiC nanowire under the circulation of gases argon by carbothermic reduction reaction.
The present invention is realized by following process：
The present invention is using metallic silicon power as silicon source in open system, and ethanol or propyl alcohol are carbon source, are prepared by carbothermic reduction reaction
Go out SiC nanowire；Specific embodiment is as follows：
1) experimental provision in open system includes：The digital injection pump and argon bottle of high temperature process furnances, liquid carbon source；
2) silica crucible for filling metallic silicon power is put into tube furnace intermediate region, and one layer is laid in the low-temperature zone of tube furnace
Graphite paper
3) in the digital injection pump of liquid carbon source and argon bottle difference inserting pipe-type stove, temperature according to required for reaction is set
Determine the heating schedule of tube furnace, and reaction soaking time is set according to the number of liquid carbon source ethanol or propyl alcohol injection volume；
4) when the temperature required for temperature reaches reaction, liquid carbon source digital injection pump is opened, carbon source ethanol or propyl alcohol are led to
Cross digital injection infusion to enter in tube furnace, and open argon bottle, liquid carbon source ethanol or propyl alcohol are gasified by Pintsch process
Tube furnace intermediate region conversion zone progress carbothermic reduction reaction is delivered to carbon source, then by argon gas；
5) after liquid carbon source injection terminates, start to start cooling process, when being down to normal temperature, laid in the low-temperature zone of tube furnace
Deposition has light green color fiber product on graphite paper.
The step 1）Open system in experimental provision be by tube furnace low-temperature end not acting flange, directly and air
Communicate and realize opening, the digital injection pump and argon bottle of liquid carbon source are to be connected with flange and communicated with tube furnace, so that real
The injection of existing liquid carbon source and the conveying of argon gas.
The step 2）Metallic silicon power, there is three kinds of different forms, silica flour by ball-milling treatment, without ball-milling treatment silicon
Powder and nanoscale silica flour；Silica flour by ball-milling treatment can reduce the grade of silica flour, increase reaction contact area.
The step 3）It is 25cm that the digital injection pump of liquid carbon source, which is connected with flange and extended in tube furnace burner hearth,
~27cm, the heating schedule that tube furnace is set is 5 DEG C/min, and temperature needed for reaction is 1500~1600 DEG C, soaking time then root
According to the number of liquid carbon source injection volume, 2~4h is set to.
The step 4）The carrier gas speed of middle argon gas is 50~300 ml/min, and the injection speed of liquid carbon source is 0.2~1
ml/min。
The step 5）In cooling process be 3 DEG C/min, low temperature depositing section graphite paper on deposition have light green color fibre
Product, is SiC nanowire.
The invention has the advantages that：
The present invention, first using lower-cost liquid ethanol or propyl alcohol as carbon source, using silica flour as silicon source, passes through under open system
Liquid carbon source is injected into tube furnace by digital injection system, is transported to the carbon source that ethanol Pintsch process is obtained instead by argon gas
Section is answered, product silicon carbide nanometer line is prepared by carbothermic reduction reaction.The present invention is realized successfully to be made under open system
Standby silicon carbide nanometer line, and can by increase the amount of silica flour and the injection volume of ethanol and extension soaking time so as to
The silicon carbide nanometer line for being expected to realize continuously is made.This method has low energy expenditure cost, and technique is simple, excellent without catalyst etc.
Point, the nano wire can apply to the fields such as enhancing ceramic matric composite, nanoelectronic senser element, photocatalysis, also simultaneously
The practical ranges of nano wire can be opened up, and present device requires low, strong operability, and experimentation is simple and suitable
Silicon carbide nanometer line is continuously prepared.
Brief description of the drawings
Fig. 1 is the schematic diagram of open system experimental provision of the present invention.
Fig. 2 is the X-ray diffractogram of the product of the embodiment of the present invention 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of the product of the embodiment of the present invention 1.
Fig. 4 is the transmission electron microscope picture of the product of the embodiment of the present invention 1.
Embodiment
Below in conjunction with drawings and examples, the present invention is further illustrated.
As shown in figure 1, the experimental provision in open system includes：The digital injection pump and argon gas of tube furnace, liquid carbon source
Bottle；The silica crucible for filling metallic silicon power is put into the tube furnace intermediate region of heating element heater, and in the low-temperature zone of tube furnace
Lay graphite paper；Experimental provision in open system is, by tube furnace low-temperature end not acting flange, realization directly to be communicated with air
Open, the digital injection pump and argon bottle of liquid carbon source are to be connected with flange and communicated with tube furnace, so as to realize liquid carbon
The injection in source and the conveying of argon gas.
Embodiment 1：
1st, using purity be 99.9% silica flour as silicon source, without ball-milling treatment, claim silica flour to be put into silica crucible, and by quartz
Crucible pushes to the intermediate region of tube furnace.And one layer of graphite paper is laid in the low-temperature zone of tube furnace, for collecting low temperature reaction
SiC nanowire obtained by deposition.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1500 DEG C, when temperature reaches 1500 DEG C, starts to be incubated 2h.
3rd, 97% ethanol 20ml is measured, is fitted into syringe, by the digital injection pump of liquid carbon source by ethanol injection to pipe
In formula stove, injection rate is 0.2ml/min, obtains carbon source by the gasification of ethanol Pintsch process, and open argon gas with 50ml/min
Carrier gas speed by crack gasification carbon source be transported to pyroreaction section, participate in reaction.
4th, after insulation 2h, normal temperature is then reduced to 3 DEG C/min again, taken out on the graphite paper of low-temperature zone laying, graphite paper
The cotton-shaped deposit of light green color is generated, is the silicon carbide nanometer line of the present invention.
As shown in Fig. 2 being the X-ray diffractogram of the product of the embodiment of the present invention 1.As shown in figure 3, being the embodiment of the present invention
The scanning electron microscope (SEM) photograph of 1 product.As shown in figure 4, being the transmission electron microscope picture of the product of the embodiment of the present invention 1.
Embodiment 2：
1st, using purity be 99.9% silica flour as silicon source, without ball-milling treatment, silica flour is put into silica crucible, and by quartz
Crucible pushes to the intermediate region of tube furnace.And one layer of graphite paper is laid in the low-temperature zone of tube furnace, for collecting low temperature reaction
SiC nanowire obtained by deposition.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1550 DEG C, when temperature reaches 1550 DEG C, starts to be incubated 2h.
3rd, the ml of 97% ethanol 50 is measured, is fitted into syringe, ethanol injection is arrived by the digital injection pump of liquid carbon source
In tube furnace, injection rate is 0.5ml/min, obtains carbon source by the gasification of ethanol Pintsch process, and open argon gas with 100ml/
The carbon source for cracking gasification is transported to pyroreaction section by min argon carrier speed, participates in reaction.
4th, step d is same as Example 1.
Embodiment 3：
1st, using purity be 99.9% silica flour as silicon source, without ball-milling treatment, silica flour is put into silica crucible, and by quartz
Crucible pushes to the intermediate region of tube furnace.And one layer of graphite paper is laid in the low-temperature zone of tube furnace, for collecting low temperature reaction
SiC nanowire obtained by deposition.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1600 DEG C, when temperature reaches 1600 DEG C, starts to be incubated 2h
3rd, the ml of 97% propyl alcohol 80 is measured, is fitted into syringe, propyl alcohol is injected into by tubular type by the digital injection pump of liquid carbon source
In stove, injection rate is 0.8ml/min, obtains carbon source by the gasification of propyl alcohol Pintsch process, and open argon gas with 300ml/min's
The carbon source for cracking gasification is transported to pyroreaction section by carrier gas speed, participates in reaction.
4th, step d is same as Example 1.
Embodiment 4：
1st, using purity be 99.9% silica flour as silicon source, silica flour is passed through into ball milling, control rotating speed be 100 r/min, Ball-milling Time
Silica flour is put into silica crucible by 0.5 h, sieving after drying, and silica crucible is pushed to the intermediate region of tube furnace.And
The low-temperature zone of tube furnace lays one layer of graphite paper, for collecting the SiC nanowire obtained by low temperature reaction deposition.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1500 DEG C, when temperature reaches 1500 DEG C, starts to be incubated 3h.
3rd, the ml of 97% ethanol 60 is measured, is fitted into syringe, ethanol injection is arrived by the digital injection pump of liquid carbon source
In tube furnace, injection rate is 0.4ml/min, obtains carbon source by the gasification of ethanol Pintsch process, and open argon gas with 180ml/
The carbon source for cracking gasification is transported to pyroreaction section by min carrier gas speed, participates in reaction.
4th, after insulation 3h, normal temperature is then reduced to 3 DEG C/min again, taken out on the graphite paper of low-temperature zone laying, graphite paper
The cotton-shaped deposit of light green color is generated, is the silicon carbide nanometer line of the present invention.
Embodiment 5：
1st, using purity be 99.9% silica flour as silicon source, silica flour is passed through into ball milling, control rotating speed be 120r/min, Ball-milling Time 1
Silica flour is put into silica crucible by h, sieving after drying, and silica crucible is pushed to the intermediate region of tube furnace.And in tubular type
The low-temperature zone of stove lays one layer of graphite paper, for collecting the SiC nanowire obtained by low temperature reaction deposition.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1550 DEG C, when temperature reaches 1550 DEG C, starts to be incubated 3h
3rd, 97% ethanol 90ml is measured, is fitted into syringe, by the digital injection pump of liquid carbon source by ethanol injection to tube furnace
Interior, injection rate is 0.6ml/min, obtains carbon source by the gasification of ethanol Pintsch process, and open argon gas with 240ml/min load
The carbon source for cracking gasification is transported to pyroreaction section by gas velocity degree, participates in reaction.
4th, step d is same as Example 4.
Embodiment 6：
1st, using purity be 99.9% silica flour as silicon source, silica flour is passed through into ball milling, control rotating speed be 150 r/min, Ball-milling Time 1
Silica flour is put into silica crucible by h, sieving after drying, and silica crucible is pushed to the intermediate region of tube furnace.And in tubular type
The low-temperature zone of stove lays one layer of graphite paper, for collecting the SiC nanowire obtained by low temperature reaction deposition.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1600 DEG C, when temperature reaches 1600 DEG C, starts to be incubated 3h.
3rd, the ml of 97% propyl alcohol 130 is measured, is fitted into syringe, propyl alcohol is injected into by the digital injection pump of liquid carbon source
In tube furnace, injection rate is 0.8ml/min, obtains carbon source by the gasification of propyl alcohol Pintsch process, and open argon gas with 300ml/
The carbon source for cracking gasification is transported to pyroreaction section by min carrier gas speed, participates in reaction.
4th, step d is same as Example 4.
Embodiment 7：
1st, using nano silica fume as silicon source, particle diameter is 20~60 nm, silica flour is put into silica crucible, and silica crucible is pushed
To the intermediate region of tube furnace.And one layer of graphite paper is laid in the low-temperature zone of tube furnace, for collecting low temperature reaction deposition gained
The SiC nanowire arrived.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1500 DEG C, when temperature reaches 1500 DEG C, starts to be incubated 4h.
3rd, the ml of 97% ethanol 40 is measured, is fitted into syringe, ethanol injection is arrived by the digital injection pump of liquid carbon source
In tube furnace, injection rate is 0.2ml/min, obtains carbon source by the gasification of ethanol Pintsch process, and open argon gas with 50ml/
The carbon source for cracking gasification is transported to pyroreaction section by min carrier gas speed, participates in reaction.
4th, after insulation 4h, normal temperature is then reduced to 3 DEG C/min again, taken out on the graphite paper of low-temperature zone laying, graphite paper
The cotton-shaped deposit of light green color is generated, is the silicon carbide nanometer line of the present invention.
Embodiment 8：
1st, using nano silica fume as silicon source, grade is 20~60 nm, silica flour is put into silica crucible, and silica crucible is pushed
To the intermediate region of tube furnace.And one layer of graphite paper is laid in the low-temperature zone of tube furnace, for collecting low temperature reaction deposition gained
The SiC nanowire arrived.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1550 DEG C, when temperature reaches 1550 DEG C, starts to be incubated 4h.
3rd, the ml of 97% ethanol 80 is measured, is fitted into syringe, ethanol injection is arrived by the digital injection pump of liquid carbon source
In tube furnace, injection rate is 0.4ml/min, obtains carbon source by the gasification of ethanol Pintsch process, and open argon gas with 160ml/
The carbon source for cracking gasification is transported to pyroreaction section by min carrier gas speed, participates in reaction.
4th, step d is same as Example 7.
Embodiment 9：
1st, using nano silica fume as silicon source, particle diameter is 20~60 nm, silica flour is put into silica crucible, and silica crucible is pushed
To the intermediate region of tube furnace.And one layer of graphite paper is laid in the low-temperature zone of tube furnace, for collecting low temperature reaction deposition gained
The SiC nanowire arrived.
2nd, the temperature setting heating schedule according to required for carbothermic reduction reaction prepares SiC nanowire, with 5 DEG C/min liter
Warm speed rises to 1600 DEG C, when temperature reaches 1600 DEG C, starts to be incubated 4h.
3rd, the ml of 97% propyl alcohol 200 is measured, is fitted into syringe, propyl alcohol is injected into by the digital injection pump of liquid carbon source
In tube furnace, injection rate is 1ml/min, obtains carbon source by the gasification of propyl alcohol Pintsch process, and open argon gas with 300ml/min
Carrier gas speed by crack gasification carbon source be transported to pyroreaction section, participate in reaction.
4th, step d is same as Example 7.
Claims (6)
1. a kind of preparation method of open system SiC nanowire, it is characterised in that：Using metallic silicon power as silicon in open system
Source, ethanol or propyl alcohol are carbon source, and SiC nanowire is prepared by carbothermic reduction reaction；Specific embodiment is as follows：
1) experimental provision in open system includes：The digital injection pump and argon bottle of tube furnace, liquid carbon source；
2) silica crucible for filling metallic silicon power is put into tube furnace intermediate region, and graphite is laid in the low-temperature zone of tube furnace
Paper；
3) in the digital injection pump of liquid carbon source and argon bottle difference inserting pipe-type stove, temperature according to required for reaction is set
Determine the heating schedule of tube furnace, and reaction soaking time is set according to the number of liquid carbon source ethanol or propyl alcohol injection volume；
4) when the temperature required for temperature reaches reaction, liquid carbon source digital injection pump is opened, carbon source ethanol or propyl alcohol are led to
Cross digital injection infusion to enter in tube furnace, and open argon bottle, liquid carbon source ethanol or propyl alcohol are gasified by Pintsch process
Tube furnace intermediate region conversion zone progress carbothermic reduction reaction is delivered to carbon source, then by argon gas；
5) after liquid carbon source injection terminates, start to start cooling process, when being down to normal temperature, laid in the low-temperature zone of tube furnace
Graphite paper on deposition have light green color fiber product.
2. a kind of preparation method of open system SiC nanowire according to claim 1, it is characterised in that：The step
1）Open system in experimental provision be by tube furnace low-temperature end not acting flange, directly communicated with air realize it is open,
The digital injection pump and argon bottle of liquid carbon source are to be connected with flange and communicated with tube furnace, so as to realize the injection of liquid carbon source
With the conveying of argon gas.
3. a kind of preparation method of open system SiC nanowire according to claim 1, it is characterised in that：The step
2）Metallic silicon power, there is three kinds of different forms, silica flour by ball-milling treatment, without ball-milling treatment silica flour and nanoscale silica flour；
Silica flour by ball-milling treatment can reduce the grade of silica flour, increase reaction contact area.
4. a kind of preparation method of open system SiC nanowire according to claim 1, it is characterised in that：The step
3）It is 25cm~27cm, tube furnace setting that the digital injection pump of liquid carbon source, which is connected with flange and extended in tube furnace burner hearth,
Heating schedule be 5 DEG C/min, reaction needed for temperature be 1500~1600 DEG C, soaking time is then according to liquid carbon source injection volume
How much, it is set to 2~4h.
5. a kind of preparation method of open system SiC nanowire according to claim 1, it is characterised in that：The step
4）The carrier gas speed of middle argon gas is 50~300 ml/min, and the injection speed of liquid carbon source is 0.2~1 ml/min.
6. a kind of preparation method of open system SiC nanowire according to claim 1, it is characterised in that：The step
Rapid 5）In cooling process be 3 DEG C/min, low temperature depositing section graphite paper on deposition have light green color fiber product, be SiC nanometers
Line.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107737943A (en) * | 2017-11-03 | 2018-02-27 | 重庆大学 | A kind of method that Reduction of methanol prepares tungsten carbide or/and tungsten powder |
| CN109437203A (en) * | 2018-11-09 | 2019-03-08 | 北京科技大学 | A kind of preparation method of high-purity one dimension SiC nano material |
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| CN102874810A (en) * | 2012-10-26 | 2013-01-16 | 浙江理工大学 | Preparation method of beta-SiC nano powder |
| US20140194278A1 (en) * | 2013-01-10 | 2014-07-10 | Korea Institute Of Science And Technology | Porous silicon carbide nanocomposite structure comprising nanowires and method of preparing the same |
| CN106119967A (en) * | 2016-06-21 | 2016-11-16 | 浙江理工大学 | Continuous two steps prepare the method for monocrystalline silicon carbide/Graphene composite nano fiber |
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| CN107737943A (en) * | 2017-11-03 | 2018-02-27 | 重庆大学 | A kind of method that Reduction of methanol prepares tungsten carbide or/and tungsten powder |
| CN107737943B (en) * | 2017-11-03 | 2019-08-02 | 重庆大学 | A kind of method that Reduction of methanol prepares tungsten carbide or/and tungsten powder |
| CN109437203A (en) * | 2018-11-09 | 2019-03-08 | 北京科技大学 | A kind of preparation method of high-purity one dimension SiC nano material |
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