CN1962433A - Silicon carbide nano line containing associated noncrystalline sphere structure and its preparation method - Google Patents
Silicon carbide nano line containing associated noncrystalline sphere structure and its preparation method Download PDFInfo
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- CN1962433A CN1962433A CN 200610151102 CN200610151102A CN1962433A CN 1962433 A CN1962433 A CN 1962433A CN 200610151102 CN200610151102 CN 200610151102 CN 200610151102 A CN200610151102 A CN 200610151102A CN 1962433 A CN1962433 A CN 1962433A
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Abstract
The invention discloses a nanometer line with associated structure and preparing method, which comprises the following parts: 6-24% carbon, 53-68% silicon and 11-40% oxygen. The preparing method comprises the following steps: (1) allocating composite gel; (2) stirring; (3) gelifing; (4) placing gel in the copple in the pipe-typed heating furnace; extracting into vacuum; (5) aerating argon gas in the pipe-typed heating furnace; (6) sintering; (7) cooling to indoor temperature to obtain the product.
Description
Technical field
The present invention relates to a kind of nano wire that has associated structure and preparation method thereof.
Background technology
In recent years, the research of SiC nano wire is in the ascendant, and the various countries scholar responds with keen interest and puts into one after another in the research of SiC nano wire, and explores the various different methods of synthetic SiC nano wire.Found the associated structure of variform under study for action, be widely used in fields such as nanometer optical cable, nanometer components and parts, opto-electronic device, the western Li Ke of Beijing Polytechnical University intelligence seminar is with SiO
2With Graphite Powder 99 be raw material, do not using the SiC nano wire that utilizes chemical Vapor deposition process yet to prepare the association ball-like structure under the condition of catalyzer, and be published in english magazine " Materials Chemistry and Physics " 95 (2006): on the 140-144, but the length of nano wire only is tens nanometers, and the little spherical diameter that association goes out is the growth that can not control ball about 1 micron effectively.
Summary of the invention
The present invention is that the nanowire length of the association ball-like structure that produces for the manufacture method that solves original association ball-like structure nano wire is short and can not control the problem of the growth of ball effectively.And a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure that provides and preparation method thereof.The SiC nano wire that contains associated noncrystalline sphere structure is made by 6～24% carbon, 53～68% silicon and 11～40% oxygen by mass percentage.The silicon carbide nanometer line that contains associated noncrystalline sphere structure prepares by following steps: (one) is 2: 1～5 the ratio preparation sucrose and the mixed sols of silicon sol according to the mol ratio of silicon and carbon; (2) mixed sols is stirred into the colloidal sol of homogeneous transparent with magnetic stirring apparatus; (3) be under 60～95 ℃ the condition colloidal sol to be carried out gelation to handle in temperature, obtain transparent or little gel that is white in color; (4) gel that obtains is put into crucible and placed atmosphere sintering furnace, vacuumize, the vacuum tightness that makes atmosphere sintering furnace is to 1Pa; (5) in atmosphere sintering furnace, charge into argon gas, make furnace gas pressure reach 0.1～2.0MPa; (6) atmosphere sintering furnace heated with the heat-up rate of 5～30 ℃/min, 1350～1700 ℃ sintering temperatures 0.5～4 hour; (7) cool to room temperature promptly obtains containing the silicon carbide nanometer line of associated noncrystalline sphere structure.The longest millimeter magnitude that reaches of association non-crystalline state globular nano wire of the present invention's preparation, the diameter of nano wire is 50～300 nanometers, nano wire is smooth straight, and association ball being evenly distributed on nano wire can be controlled at the diameter of ball in 0.5～20 micron the scope by regulating processing parameter; Product contains ball-like structure and helps obtaining combination of better interface and toughening effect, thereby is used for the enhancing of ceramic composite, metal composite better, is a kind of ideal composite material reinforcement body.
Description of drawings
Fig. 1 is 100 times of electron microscope scanning figure of SiC nano wire of the association non-crystalline state bead of embodiment three preparation, and Fig. 2 is 1000 times of electron microscope scanning figure of SiC nano wire of the association non-crystalline state bead of embodiment three preparations.
Embodiment
Embodiment one: the silicon carbide nanometer line that contains associated noncrystalline sphere structure of present embodiment is made up of carbon and silicon, and it is made by 6～24% carbon, 53～68% silicon and 11～40% oxygen by mass percentage.
Embodiment two: the silicon carbide nanometer line that the difference of present embodiment and embodiment one is to contain associated noncrystalline sphere structure is made by 7～23% carbon, 54～65% silicon and 12～39% oxygen by mass percentage.
Embodiment three: present embodiment realizes a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure of preparation by following steps: (one) is the mixed sols that 2: 1～5 ratio is prepared sucrose and silicon sol according to the mol ratio of silicon and carbon; (2) mixed sols is stirred into the colloidal sol of homogeneous transparent with magnetic stirring apparatus; (3) be under 60～95 ℃ the condition colloidal sol to be carried out gelation to handle in temperature, obtain transparent or little gel that is white in color; (4) gel that obtains is put into crucible and placed atmosphere sintering furnace, vacuumize, the vacuum tightness that makes atmosphere sintering furnace is to 1Pa; (5) in atmosphere sintering furnace, charge into argon gas, make furnace gas pressure reach 0.1～2.0MPa; (6) atmosphere sintering furnace heated with the heat-up rate of 5～30 ℃/min, 1350～1700 ℃ sintering temperatures 0.5～4 hour; (7) cool to room temperature promptly obtains containing the silicon carbide nanometer line of associated noncrystalline sphere structure.
The silicon carbide nanometer line electron microscope observation that contains associated noncrystalline sphere structure of present embodiment preparation, 100 times of scanning results such as Fig. 1,1000 times of scanning results are shown in Figure 2, among Fig. 1, Fig. 2 the silicon carbide bead with the non-crystalline state form have, be of a size of micron dimension, be distributed in 0.5～20 micron the scope, be evenly distributed on the SiC nano wire, little sphere gap is basic identical and present periodically.
Embodiment four: the difference of present embodiment and embodiment three is that the mol ratio according to silicon and carbon is 2: 4 the ratio preparation sucrose and the mixed sols of silicon sol in the step ().Other step is identical with embodiment three.
Embodiment five: the difference of present embodiment and embodiment three is that under 90 ℃ of temperature condition mixed sols being carried out gelation in the step (three) handles.Other step is identical with embodiment three.
Embodiment six: the difference of present embodiment and embodiment three is to make furnace gas pressure reach 0.5Mpa in the step (five).Other step is identical with embodiment three.
Embodiment seven: the difference of present embodiment and embodiment three is to make furnace gas pressure reach 1.0Mpa in the step (five).Other step is identical with embodiment three.
Embodiment eight: the difference of present embodiment and embodiment three is that sintering time is 2 hours in the step (six).Other step is identical with embodiment three.
Embodiment nine: the difference of present embodiment and embodiment three is to carry out in the step (six) atmosphere sintering under 1500 ℃ temperature.Other step is identical with embodiment three.
Embodiment ten: the difference of present embodiment and embodiment three is to carry out in the step (six) atmosphere sintering under 1600 ℃ temperature.Other step is identical with embodiment three.
Embodiment 11: the difference of present embodiment and embodiment three is in the step (seven) cool to room temperature in cooling water recirculation system.Other step is identical with embodiment three.
Claims (10)
1, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure, the SiC nano wire that it is characterized in that containing associated noncrystalline sphere structure are made by 6～24% carbon, 53～68% silicon and 11～40% oxygen by mass percentage.
2, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure according to claim 1, the SiC nano wire that it is characterized in that containing associated noncrystalline sphere structure are made by 7～23% carbon, 54～65% silicon and 12～39% oxygen by mass percentage.
3, a kind of preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure is characterized in that the silicon carbide nanometer line that contains associated noncrystalline sphere structure prepares by following steps: (one) is 2: 1～5 the ratio preparation sucrose and the mixed sols of silicon sol according to the mol ratio of silicon and carbon; (2) mixed sols is stirred into the colloidal sol of homogeneous transparent with magnetic stirring apparatus; (3) be under 60～95 ℃ the condition colloidal sol to be carried out gelation to handle in temperature, obtain transparent or little gel that is white in color; (4) gel that obtains is put into crucible and placed atmosphere sintering furnace, vacuumize, the vacuum tightness that makes atmosphere sintering furnace is to 1Pa; (5) in atmosphere sintering furnace, charge into argon gas, make furnace gas pressure reach 0.1～2.0MPa; (6) atmosphere sintering furnace heated with the heat-up rate of 5～30 ℃/min, 1350～1700 ℃ sintering temperatures 0.5～4 hour; (7) cool to room temperature promptly obtains containing the silicon carbide nanometer line of associated noncrystalline sphere structure.
4, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure according to claim 3 and preparation method thereof is characterized in that the mol ratio according to silicon and carbon is 2: 4 the ratio preparation sucrose and the mixed sols of silicon sol in the step ().
5, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure according to claim 3 and preparation method thereof is characterized in that under 90 ℃ of temperature condition mixed sols being carried out gelation in the step (three) handles.
6, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure according to claim 3 and preparation method thereof is characterized in that making furnace gas pressure reach 0.5Mpa in the step (five).
7, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure according to claim 3 and preparation method thereof is characterized in that making furnace gas pressure reach 1.0Mpa in the step (five).
8, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure according to claim 3 and preparation method thereof is characterized in that sintering time is 2 hours in the step (six).
9, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure according to claim 3 and preparation method thereof is characterized in that carrying out in the step (six) atmosphere sintering under 1500 ℃ temperature.
10, a kind of silicon carbide nanometer line that contains associated noncrystalline sphere structure according to claim 3 and preparation method thereof is characterized in that carrying out in the step (six) atmosphere sintering under 1600 ℃ temperature.
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| CNB2006101511029A CN100467374C (en) | 2006-12-06 | 2006-12-06 | Silicon carbide nano line containing associated noncrystalline sphere structure and its preparation method |
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| CNB2006101511029A CN100467374C (en) | 2006-12-06 | 2006-12-06 | Silicon carbide nano line containing associated noncrystalline sphere structure and its preparation method |
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| CN100467374C CN100467374C (en) | 2009-03-11 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102195037A (en) * | 2010-03-05 | 2011-09-21 | 张少波 | Method for preparing nanocrystalline silicon carbide/amorphous silicon carbide/graphite composite anode material |
| CN102195031A (en) * | 2010-03-05 | 2011-09-21 | 张少波 | Method for preparing nano-wire silicon carbide/graphite composite cathode materials of lithium-ion batteries at high temperature |
| CN106673708A (en) * | 2016-12-02 | 2017-05-17 | 西北工业大学 | Method for preparing silicon carbide nanowire porous layer on surface of carbon/carbon composite material |
| CN113666375A (en) * | 2021-09-06 | 2021-11-19 | 常州大学 | Green preparation method of beta-silicon carbide with high specific surface area |
-
2006
- 2006-12-06 CN CNB2006101511029A patent/CN100467374C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102195037A (en) * | 2010-03-05 | 2011-09-21 | 张少波 | Method for preparing nanocrystalline silicon carbide/amorphous silicon carbide/graphite composite anode material |
| CN102195031A (en) * | 2010-03-05 | 2011-09-21 | 张少波 | Method for preparing nano-wire silicon carbide/graphite composite cathode materials of lithium-ion batteries at high temperature |
| CN106673708A (en) * | 2016-12-02 | 2017-05-17 | 西北工业大学 | Method for preparing silicon carbide nanowire porous layer on surface of carbon/carbon composite material |
| CN106673708B (en) * | 2016-12-02 | 2019-07-05 | 西北工业大学 | A kind of method that surface of carbon/carbon composite prepares silicon carbide nanometer line porous layer |
| CN113666375A (en) * | 2021-09-06 | 2021-11-19 | 常州大学 | Green preparation method of beta-silicon carbide with high specific surface area |
| CN113666375B (en) * | 2021-09-06 | 2023-10-27 | 常州大学 | Green preparation method of beta-silicon carbide with high specific surface area |
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| CN100467374C (en) | 2009-03-11 |
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