CN103318891B - Method for generating one-dimensional silicon carbide nanowires on multiporous charcoal template - Google Patents
Method for generating one-dimensional silicon carbide nanowires on multiporous charcoal template Download PDFInfo
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- CN103318891B CN103318891B CN201310284190.XA CN201310284190A CN103318891B CN 103318891 B CN103318891 B CN 103318891B CN 201310284190 A CN201310284190 A CN 201310284190A CN 103318891 B CN103318891 B CN 103318891B
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- silicon carbide
- charcoal template
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- biological charcoal
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Abstract
The invention particularly relates to a preparation method for generating one-dimensional silicon carbide nanowires on a multiporous charcoal template. According to the technical scheme, the preparation method comprises the following steps of: mixing 20-40wt% of a silicon source-containing substance and 60-80wt% of industrial-grade salt for 10-60 minutes on a planetary ball mill, and then drying for 12 hours on the condition of 110 DEG C, so as to prepare a mixed powder; then placing the multiporous charcoal template in the mixed powder, insulting heat for 2-10 hours in an argon atmosphere on the condition of 1250-1400 DEG C, and naturally cooling; and finally using water as a solvent for dissolving out salt, so as to obtain the one-dimensional silicon carbide nanowires on the multiporous charcoal template. The method disclosed by the invention has the characteristics of abundant raw materials, low production cost, simple process and easiness in industrialized production, and the recovered salt can be repeatedly utilized; and the one-dimensional silicon carbide nanowires generated on the multiporous charcoal template by the method are good in crystal morphology and high in phase purity.
Description
Technical field
The invention belongs to one dimension silicon carbide nanometer line technical field, be specifically related to a kind of method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
Background technology
Natural log has unique cellularstructure, and different types of wood structure is also different, aboundresources, and renewable, price is also cheap.Log is the charcoal mould material that obtains after charing, remains the original microstructure of log to a certain extent, has high porosity, unidirectional through hole, unimodal or multi-modal pore size distribution, hole table be easy to modification and the feature such as microstructure and Mechanical Property Anisotropy.In biomimetic material research, bionic structure is a hot research direction, the composite organic-inorganic material tool utilizing charcoal template to carry out designing and preparing special construction and performance is of great significance, utilize this structure can prepare support of the catalyst, advanced microreactor, the fixer of viable cell, Heat retaining and insulation material and high-temperature filter etc., have broad application prospects.But the oxidation-resistance of charcoal template is poor, limited to the contact area of catalyzer, limits its application to a certain extent.
Molten-salt synthesis adopts the salt of one or several low melting points as reaction medium usually, and reactant has certain solubleness in fused salt, and reaction is carried out in atom level.After reaction terminates, adopt suitable solvent to be dissolved by salt, can synthetic product be obtained after washing after filtration.
Because low melting point salt is as reaction medium, have liquid phase to occur in building-up process, reactant has certain solubleness wherein, greatly accelerates the rate of diffusion of ion, make reactant realize atomic scale mixing in the liquid phase, reaction is just converted into solid-liquid reaction by solid-solid reaction.
In existing research method, mostly adopt sol-gel method and carbothermic method to prepare biological stephanoporate stupalith, as sol-gel method the cost of material that uses costly, and be organism mostly, to health and the bad environmental of people, experimental period is longer.And use carbothermic method, owing to being solid-solid reaction, not only firing temperature is higher, and destroys the biological structure of charcoal template to a certain extent.
Summary of the invention
The present invention is intended to overcome prior art defect, and object is to provide a kind of abundant raw material, production cost is low, technique is simple and be easy to the method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template of suitability for industrialized production.
For achieving the above object, the technical solution adopted in the present invention is: first the siliceous source material of 20 ~ 40wt% and the technical grade salt of 60 ~ 80wt% are mixed on planetary ball mill, mix 10 ~ 60 minutes, then under the condition of 110 DEG C dry 12 hours, obtained mixed powder.Then multiporous biological charcoal template is inserted in mixed powder, under argon gas atmosphere and 1250 ~ 1400 DEG C of conditions be incubated 2 ~ 10 hours, naturally cooling, with water be finally solvent by salt stripping, obtain generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
Described siliceous source material is SiO
2powder or be Si powder; SiO
2the particle diameter of powder and Si powder is less than 20 μm, Si powder and SiO
2purity>=the 90wt% of powder.
Described technical grade salt is the mixture of NaF and NaCl or the mixture for KF and NaCl; Wherein, the purity >=99wt% of NaCl powder, NaF and KF.
The preparation method of described multiporous biological charcoal template is: first insert in tube furnace by log, be warmed up to 600 ~ 800 DEG C under inert atmosphere protection, is incubated 1 ~ 3 hour; And then be warming up to 900 ~ 1200 DEG C, be incubated 1 ~ 3 hour, furnace cooling, obtained multiporous biological charcoal template.
Described purity of argon > 99wt%.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
Silicon source of the present invention material, multiporous biological charcoal template and Industrial Salt wide material sources, production cost is low.
The present invention is in preparation process, first by silicon source material and technical grade salt mix grinding, dry, and burn till at 1250 ~ 1400 DEG C, cooling is finally that solvent is by salt stripping with water.Therefore preparation technology is simple, synthesis temperature is low, and soaking time is short, and salt is easily separated and can reuse, and is easy to suitability for industrialized production.
The one dimension silicon carbide nanometer line crystal morphology that the present invention grows in multiporous biological charcoal template is good, and thing phase purity is high, and the diameter of its nano wire is 10 ~ 90nm, structural integrity and rule.Experiment proves, the quantity of the one dimension silicon carbide nanometer line that multiporous biological charcoal template grows, length and pattern are along with ratio different and different of firing temperature and raw material; Multiporous biological charcoal template prepared by the present invention maintains the original microstructure of log.
Therefore, the present invention not only has abundant raw material, production cost is low, technique is simple and be easy to the feature of suitability for industrialized production, and the salt reclaimed can reuse; In multiporous biological charcoal template, generate by the method that one dimension silicon carbide nanometer line crystal morphology is good and thing phase purity is high.
Accompanying drawing explanation
Fig. 1 is a kind of SEM photo generating one dimension silicon carbide nanometer line in multiporous biological charcoal template of the present invention;
Fig. 2 is for generating the SEM photo in the multiporous biological charcoal template described in Fig. 1 prepared by product.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described, the restriction not to its protection domain.
For avoiding repetition, first by as follows to the preparation of the multiporous biological charcoal template involved by this embodiment, silicon source material and technical grade salt Unify legislation, repeat no more in embodiment:
SiO
2the particle diameter of powder and Si powder is less than 20 μm, Si powder and SiO
2purity>=the 90wt% of powder;
Purity >=99 wt% of described NaCl powder, NaF powder and KF powder; Described purity of argon > 99wt%.；
The preparation method of described multiporous biological charcoal template is: first insert in tube furnace by log, be warmed up to 600 ~ 800 DEG C under inert atmosphere protection, is incubated 1 ~ 3 hour; And then be warming up to 900 ~ 1200 DEG C, be incubated 1 ~ 3 hour, furnace cooling, obtained multiporous biological charcoal template.
embodiment 1
A kind of method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
First the siliceous source material of 20 ~ 30wt% and the technical grade salt of 70 ~ 80wt% are mixed on planetary ball mill, mix 10 ~ 30 minutes, then under the condition of 110 DEG C dry 12 hours, obtained mixed powder.Then multiporous biological charcoal template is inserted in mixed powder, under argon gas atmosphere and 1250 ~ 1350 DEG C of conditions be incubated 8 ~ 10 hours, naturally cooling, with water be finally solvent by salt stripping, obtain generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: siliceous source material is Si powder; Technical grade salt is the mixture of NaF and NaCl, and wherein the mass ratio of NaCl ︰ NaF is 10 ︰ (0.1 ~ 2).
embodiment 2
A kind of method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
First the siliceous source material of 30 ~ 40wt% and the technical grade salt of 60 ~ 70wt% are mixed on planetary ball mill, mix 30 ~ 60 minutes, then under the condition of 110 DEG C dry 12 hours, obtained mixed powder.Then multiporous biological charcoal template is inserted in mixed powder, under argon gas atmosphere and 1350 ~ 1400 DEG C of conditions be incubated 2 ~ 8 hours, naturally cooling, with water be finally solvent by salt stripping, obtain generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: siliceous source material is Si powder; Technical grade salt is the mixture of KF and NaCl, and wherein the mass ratio of NaCl ︰ KF is 10 ︰ (0.1 ~ 2).
embodiment 3
A kind of method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: silica removal source material is SiO
2outside powder, all the other are with example 1.
embodiment 4
A kind of method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: except technical grade salt, all the other are with example 1, the technical grade salt described in the present embodiment is the mixture of KF and NaCl, and wherein the mass ratio of NaCl ︰ KF is 10 ︰ (0.1 ~ 2).
embodiment 5
A kind of method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: silica removal source material is SiO
2outside powder, all the other are with example 2.
embodiment 6
A kind of method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: except technical grade salt, all the other are with example 2, the technical grade salt described in the present embodiment is the mixture of NaF and NaCl, and wherein the mass ratio of NaCl ︰ NaF is 10 ︰ (0.1 ~ 2).
This embodiment compared with prior art, has following positively effect:
Silicon source material, charcoal template and Industrial Salt wide material sources that this embodiment adopts, production cost is low;
This embodiment is in preparation process, first by silicon source material and technical grade salt mix grinding, dry, and burn till at 1250 ~ 1400 DEG C, cooling is finally that solvent is by salt stripping with water.Therefore preparation technology is simple, synthesis temperature is low, and soaking time is short, and salt is easily separated and can reuse, and is easy to suitability for industrialized production.
Fig. 1 is the one growth of one-dimensional silicon carbide nanometer line in multiporous biological charcoal template in this embodiment, and crystal morphology is good, and thing phase purity is high, and the diameter of its nano wire is 10 ~ 90nm, structural integrity and rule.Multiporous biological charcoal template prepared by this embodiment as shown in Figure 2, maintains the original microstructure of log.The experiment of this embodiment proves, the quantity of one dimension silicon carbide nanometer line, length, pattern are along with ratio different and different of firing temperature and raw material
Therefore, this embodiment not only has abundant raw material, production cost is low, technique is simple and be easy to the feature of suitability for industrialized production, and the salt reclaimed can reuse; In multiporous biological charcoal template, generate by the method that one dimension silicon carbide nanometer line crystal morphology is good and thing phase purity is high.
Claims (3)
1. one kind generates the method for one dimension silicon carbide nanometer line in multiporous biological charcoal template, first the siliceous source material of 20 ~ 40wt% and the technical grade salt of 60 ~ 80wt% are mixed on planetary ball mill, mix 10 ~ 60 minutes, then under the condition of 110 DEG C dry 12 hours, obtained mixed powder; Then multiporous biological charcoal template is inserted in mixed powder, under argon gas atmosphere and 1250 ~ 1400 DEG C of conditions be incubated 2 ~ 10 hours, naturally cooling, with water be finally solvent by salt stripping, obtain generating one dimension silicon carbide nanometer line in multiporous biological charcoal template;
Described siliceous source material is SiO
2powder or be Si powder; SiO
2the particle diameter of powder and Si powder is less than 20 μm, Si powder and SiO
2purity>=the 90wt% of powder;
Described technical grade salt is the mixture of NaF powder and NaCl powder or the mixture for KF powder and NaCl powder; Wherein, the purity >=99wt% of NaCl powder, NaF powder and KF powder.
2. the method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template according to claim 1, it is characterized in that the preparation method of described multiporous biological charcoal template is: first insert in tube furnace by log, under inert atmosphere protection, be warmed up to 600 ~ 800 DEG C, be incubated 1 ~ 3 hour; And then be warming up to 900 ~ 1200 DEG C, be incubated 1 ~ 3 hour, furnace cooling, obtained multiporous biological charcoal template.
3. the method generating one dimension silicon carbide nanometer line in multiporous biological charcoal template according to claim 1, is characterized in that described purity of argon > 99wt%.
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| CN103318891B true CN103318891B (en) | 2015-01-28 |
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| CN105129802B (en) * | 2015-08-19 | 2017-10-20 | 常州大学 | A kind of preparation method of nanometer silicon carbide piece |
| CN105036136B (en) * | 2015-08-19 | 2018-01-02 | 常州大学 | A kind of preparation method of nanometer silicon carbide porous material |
| CN109320277B (en) * | 2018-11-16 | 2021-10-19 | 江苏科技大学 | Preparation method of SiCnw/C nano composite material |
| CN115246646B (en) * | 2021-12-22 | 2023-12-29 | 浙江理工大学 | Method for preparing silicon carbide nanowires by using renewable resources or wastes as carbon |
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| CN1268580C (en) * | 2002-12-27 | 2006-08-09 | 石油大学(北京) | Method for preparing SIC micro nano ceramic powder via refinery coke salt bath synthesis |
| CN100593512C (en) * | 2008-06-24 | 2010-03-10 | 陕西科技大学 | Method for synthesizing beta-SiC nano-wire |
| CN101746759B (en) * | 2010-02-11 | 2012-07-25 | 浙江工业大学 | Method for synthesizing silicon carbide nano wire by utilizing plant fiber |
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