CN103318891A - 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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- CN103318891A CN103318891A CN201310284190XA CN201310284190A CN103318891A CN 103318891 A CN103318891 A CN 103318891A CN 201310284190X A CN201310284190X A CN 201310284190XA CN 201310284190 A CN201310284190 A CN 201310284190A CN 103318891 A CN103318891 A CN 103318891A
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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 that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
Background technology
Natural log has unique cellularstructure, and different types of wood structure also has nothing in common with each other, aboundresources, and renewable, price is also cheap.The charcoal mould material of log through obtaining after the charing kept the original microstructure of log to a certain extent, has high porosity, unidirectional through hole, unimodal or multimodal pore size distribution, the hole table is easy to modification and features such as microstructure and mechanical property anisotropy.In biomimetic material research, bionic structure is a hot research direction, the composite organic-inorganic material that utilizes the charcoal template to design and prepare special construction and performance has very important meaning, utilize this structure can prepare fixer, insulation and the lagging material of support of the catalyst, advanced microreactor, viable cell and high-temperature filter etc., have broad application prospects.But the oxidation-resistance of charcoal template is relatively poor, limited to the contact area of catalyzer, has limited its application to a certain extent.
The fused salt synthesis method usually adopt a kind of or several low-melting salts as reaction medium, reactant has certain solubleness in fused salt, make that being reflected at atom level carries out.Reaction adopts suitable solvent that salt is dissolved after finishing, and can obtain synthetic product after the washing after filtration.
Because low melting point salt is as reaction medium, have liquid phase to occur in the building-up process, reactant has certain solubleness therein, has accelerated the rate of diffusion of ion greatly, make reactant realize that in liquid phase atomic scale mixes, reaction just is converted into solid-liquid reaction by solid-solid reaction.
In existing research method, adopt sol-gel method and carbothermic method to prepare the biological stephanoporate stupalith mostly, relatively more expensive as the employed cost of material of sol-gel method, and be organism mostly, harmful to people's health and environment, experimental period is long etc.And the use carbothermic method, owing to be solid-solid reaction, not only firing temperature is higher, and has destroyed the biological structure of charcoal template to a certain extent.
Summary of the invention
The present invention is intended to overcome the prior art defective, purpose provides a kind of abundant raw material, production cost is low, technology is simple and be easy to suitability for industrialized production generate the method for one dimension silicon carbide nanometer line in multiporous biological charcoal template.
For achieving the above object, the technical solution adopted in the present invention is: earlier the siliceous source material of 20 ~ 40wt% and the technical grade salt of 60 ~ 80wt% are mixed at planetary ball mill, mixed 10 ~ 60 minutes, and under 110 ℃ condition dry 12 hours again, made mixed powder.Then multiporous biological charcoal template is inserted in the mixed powder, under argon gas atmosphere and 1250 ~ 1400 ℃ of conditions, is incubated 2 ~ 10 hours, naturally cooling, with water be at last solvent with the salt stripping, obtain generating the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
Described siliceous source material is SiO
2Powder or be the Si powder; SiO
2The particle diameter of powder and Si powder is less than 20 μ m, Si powder and SiO
2Purity 〉=the 90wt% of powder.
The mixture that described technical grade salt is NaF and NaCl or be the mixture of KF and NaCl; Wherein, purity 〉=99wt% of NaCl powder, NaF and KF.
The preparation method of described multiporous biological charcoal template is: earlier log is inserted in the tube furnace, be warmed up to 600 ~ 800 ℃ under inert atmosphere protection, be incubated 1 ~ 3 hour; And then be warming up to 900 ~ 1200 ℃, and being incubated 1 ~ 3 hour, furnace cooling makes multiporous biological charcoal template.
Described purity of argon＞99wt%.
Because adopt technique scheme, the present invention compared with prior art has following positively effect:
Silicon of the present invention source material, multiporous biological charcoal template and Industrial Salt wide material sources, production cost is low.
The present invention is in preparation process, and earlier with silicon source material and technical grade salt mix grinding, drying is burnt till at 1250 ~ 1400 ℃, and cooling is that solvent is with the salt stripping at last with water.So 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, thing phase purity height, and the diameter of its nano wire is 10 ~ 90nm, structural integrity and rule.Quantity, length and the pattern that experiment showed, the one dimension silicon carbide nanometer line of growing in multiporous biological charcoal template is along with the ratio of firing temperature and raw material is different and different; The prepared multiporous biological charcoal template of the present invention has kept the original microstructure of log.
Therefore, the present invention not only has abundant raw material, production cost is low, technology is simple and be easy to the characteristics of suitability for industrialized production, and the salt that reclaims can reuse; With this method multiporous biological charcoal template generate one dimension silicon carbide nanometer line crystal morphology good with thing purity height mutually.
Description of drawings
Fig. 1 is a kind of SEM photo that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template of the present invention;
Fig. 2 is for generating the SEM photo on the prepared multiporous biological charcoal template of the described product of Fig. 1.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments, is not the restriction to its protection domain.
For avoiding repetition, preparation, silicon source material and the unification of technical grade salt of earlier that this embodiment is related multiporous biological charcoal template are described below, and repeat no more among the embodiment:
SiO
2The particle diameter of powder and Si powder is less than 20 μ m, Si powder and SiO
2Purity 〉=the 90wt% of powder;
The purity of described NaCl powder, NaF powder and KF powder 〉=99 wt%; Described purity of argon＞99wt%.；
The preparation method of described multiporous biological charcoal template is: earlier log is inserted in the tube furnace, be warmed up to 600 ~ 800 ℃ under inert atmosphere protection, be incubated 1 ~ 3 hour; And then be warming up to 900 ~ 1200 ℃, and being incubated 1 ~ 3 hour, furnace cooling makes multiporous biological charcoal template.
Embodiment 1
A kind of method that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
Earlier the siliceous source material of 20 ~ 30wt% and the technical grade salt of 70 ~ 80wt% are mixed at planetary ball mill, mixed 10 ~ 30 minutes, drying 12 hours under 110 ℃ condition makes mixed powder again.Then multiporous biological charcoal template is inserted in the mixed powder, under argon gas atmosphere and 1250 ~ 1350 ℃ of conditions, is incubated 8 ~ 10 hours, naturally cooling, with water be at last solvent with the salt stripping, obtain generating the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: siliceous source material is the 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 that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
Earlier the siliceous source material of 30 ~ 40wt% and the technical grade salt of 60 ~ 70wt% are mixed at planetary ball mill, mixed 30 ~ 60 minutes, drying 12 hours under 110 ℃ condition makes mixed powder again.Then multiporous biological charcoal template is inserted in the mixed powder, under argon gas atmosphere and 1350 ~ 1400 ℃ of conditions, is incubated 2 ~ 8 hours, naturally cooling, with water be at last solvent with the salt stripping, obtain generating the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: siliceous source material is the 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 that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: silica removal source material is SiO
2Outside the powder, all the other are with example 1.
A kind of method that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: except technical grade salt all the other with example 1, the mixture that the described technical grade salt of present embodiment is KF and NaCl, wherein the mass ratio of NaCl ︰ KF is 10 ︰ (0.1 ~ 2).
Embodiment 5
A kind of method that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: silica removal source material is SiO
2Outside the powder, all the other are with example 2.
Embodiment 6
A kind of method that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
In the present embodiment: except technical grade salt all the other with example 2, the mixture that the described technical grade salt of present embodiment is NaF and NaCl, 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, and earlier with silicon source material and technical grade salt mix grinding, drying is burnt till at 1250 ~ 1400 ℃, and cooling is that solvent is with the salt stripping at last with water.So 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 a kind of in this embodiment growth of one-dimensional silicon carbide nanometer line on multiporous biological charcoal template, and crystal morphology is good, thing phase purity height, and the diameter of its nano wire is 10 ~ 90nm, structural integrity and rule.The multiporous biological charcoal template of this embodiment preparation has kept the original microstructure of log as shown in Figure 2.The quantity that experiment showed, the one dimension silicon carbide nanometer line of this embodiment, length, pattern are along with the ratio of firing temperature and raw material is different and different
Therefore, this embodiment not only has abundant raw material, production cost is low, technology is simple and be easy to the characteristics of suitability for industrialized production, and the salt that reclaims can reuse; With this method multiporous biological charcoal template generate one dimension silicon carbide nanometer line crystal morphology good with thing purity height mutually.
Claims (5)
1. method that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template, earlier the siliceous source material of 20 ~ 40wt% and the technical grade salt of 60 ~ 80wt% are mixed at planetary ball mill, mixed 10 ~ 60 minutes, and under 110 ℃ condition dry 12 hours again, made mixed powder; Then multiporous biological charcoal template is inserted in the mixed powder, under argon gas atmosphere and 1250 ~ 1400 ℃ of conditions, is incubated 2 ~ 10 hours, naturally cooling, with water be at last solvent with the salt stripping, obtain generating the one dimension silicon carbide nanometer line in multiporous biological charcoal template.
2. the method at multiporous biological charcoal template generation one dimension silicon carbide nanometer line according to claim 1 is characterized in that described siliceous source material is SiO
2Powder or be the Si powder; SiO
2The particle diameter of powder and Si powder is less than 20 μ m, Si powder and SiO
2Purity 〉=the 90wt% of powder.
3. the method at multiporous biological charcoal template generation one dimension silicon carbide nanometer line according to claim 1 is characterized in that described technical grade salt is the mixture of NaF powder and NaCl powder or is the mixture of KF powder and NaCl powder; Wherein, the purity 〉=99wt% of NaCl powder, NaF powder and KF powder.
4. the method that generates the one dimension silicon carbide nanometer line in multiporous biological charcoal template according to claim 1, the preparation method who it is characterized in that described multiporous biological charcoal template is: earlier log is inserted in the tube furnace, under inert atmosphere protection, be warmed up to 600 ~ 800 ℃, be incubated 1 ~ 3 hour; And then be warming up to 900 ~ 1200 ℃, and being incubated 1 ~ 3 hour, furnace cooling makes multiporous biological charcoal template.
5. the method at multiporous biological charcoal template generation one dimension silicon carbide nanometer line according to claim 1 is characterized in that described purity of argon＞99wt%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036136A (en) * | 2015-08-19 | 2015-11-11 | 常州大学 | Preparation method of silicon carbide nano porous material |
| CN105129802A (en) * | 2015-08-19 | 2015-12-09 | 常州大学 | Preparation method for silicon carbide nanosheet |
| CN109320277A (en) * | 2018-11-16 | 2019-02-12 | 江苏科技大学 | A kind of preparation method of SiCnw/C nanocomposite |
| CN115246646A (en) * | 2021-12-22 | 2022-10-28 | 浙江理工大学 | Method for preparing silicon carbide nano-wire by using renewable resources or wastes as carbon source |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511807A (en) * | 2002-12-27 | 2004-07-14 | 石油大学(北京) | Method for preparing SIC micro nano ceramic powder via refinery coke salt bath synthesis |
| CN101306816A (en) * | 2008-06-24 | 2008-11-19 | 陕西科技大学 | Method for synthesizing beta-SiC nano-wire |
| CN101746759A (en) * | 2010-02-11 | 2010-06-23 | 浙江工业大学 | Method for synthesizing silicon carbide nano wire by utilizing plant fiber |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511807A (en) * | 2002-12-27 | 2004-07-14 | 石油大学(北京) | Method for preparing SIC micro nano ceramic powder via refinery coke salt bath synthesis |
| CN101306816A (en) * | 2008-06-24 | 2008-11-19 | 陕西科技大学 | Method for synthesizing beta-SiC nano-wire |
| CN101746759A (en) * | 2010-02-11 | 2010-06-23 | 浙江工业大学 | Method for synthesizing silicon carbide nano wire by utilizing plant fiber |
Non-Patent Citations (1)
| Title |
|---|
| WEI XIE,ET AL.: "Molten salt synthesis of silicon carbide nanorods using carbon nanotubes as templates", 《JOURNAL OF MATERIALS CHEMISTRY》, vol. 21, 14 October 2011 (2011-10-14), pages 18325 - 18330 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036136A (en) * | 2015-08-19 | 2015-11-11 | 常州大学 | Preparation method of silicon carbide nano porous material |
| CN105129802A (en) * | 2015-08-19 | 2015-12-09 | 常州大学 | Preparation method for silicon carbide nanosheet |
| CN109320277A (en) * | 2018-11-16 | 2019-02-12 | 江苏科技大学 | A kind of preparation method of SiCnw/C nanocomposite |
| CN109320277B (en) * | 2018-11-16 | 2021-10-19 | 江苏科技大学 | Preparation method of SiCnw/C nano composite material |
| CN115246646A (en) * | 2021-12-22 | 2022-10-28 | 浙江理工大学 | Method for preparing silicon carbide nano-wire by using renewable resources or wastes as carbon source |
| 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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