CN100467374C - 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
- Publication number
- CN100467374C CN100467374C CNB2006101511029A CN200610151102A CN100467374C CN 100467374 C CN100467374 C CN 100467374C CN B2006101511029 A CNB2006101511029 A CN B2006101511029A CN 200610151102 A CN200610151102 A CN 200610151102A CN 100467374 C CN100467374 C CN 100467374C
- Authority
- CN
- China
- Prior art keywords
- noncrystalline
- preparation
- silicon carbide
- sphere structure
- nanometer line
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Ceramic Products (AREA)
- Carbon And Carbon Compounds (AREA)
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 preparation method who has the nano wire of associated structure.
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 preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure who provides.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 the ratio preparation sucrose of 2:1～5 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 ratio preparation sucrose of 2:1～5 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 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 the ratio preparation sucrose of 2:4 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 (8)
1, 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 the ratio preparation sucrose of 2:1～5 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.
2, a kind of preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure according to claim 1 is characterized in that the mol ratio according to silicon and carbon is the ratio preparation sucrose of 2:4 and the mixed sols of silicon sol in the step ().
3, a kind of preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure according to claim 1 is characterized in that under 90 ℃ of temperature condition mixed sols being carried out gelation in the step (three) handles.
4, a kind of preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure according to claim 1 is characterized in that making furnace gas pressure reach 0.5Mpa in the step (five).
5, a kind of preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure according to claim 1 is characterized in that making furnace gas pressure reach 1.0Mpa in the step (five).
6, a kind of preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure according to claim 1 is characterized in that sintering time is 2 hours in the step (six).
7, a kind of preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure according to claim 1 is characterized in that carrying out in the step (six) atmosphere sintering under 1500 ℃ temperature.
8, a kind of preparation method who contains the silicon carbide nanometer line of associated noncrystalline sphere structure according to claim 1 is characterized in that carrying out in the step (six) atmosphere sintering under 1600 ℃ temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101511029A CN100467374C (en) | 2006-12-06 | 2006-12-06 | Silicon carbide nano line containing associated noncrystalline sphere structure and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101511029A CN100467374C (en) | 2006-12-06 | 2006-12-06 | Silicon carbide nano line containing associated noncrystalline sphere structure and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1962433A CN1962433A (en) | 2007-05-16 |
| CN100467374C true CN100467374C (en) | 2009-03-11 |
Family
ID=38081689
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101511029A Expired - Fee Related CN100467374C (en) | 2006-12-06 | 2006-12-06 | Silicon carbide nano line containing associated noncrystalline sphere structure and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100467374C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102195037A (en) * | 2010-03-05 | 2011-09-21 | 张少波 | Method for preparing nanocrystalline silicon carbide/amorphous silicon carbide/graphite composite anode 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 |
| CN113666375B (en) * | 2021-09-06 | 2023-10-27 | 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
Non-Patent Citations (4)
| Title |
|---|
| 一种碳化硅纳米线的合成方法. 陈静.淮阴工学院学报，第15卷第3期. 2006 |
| 一种碳化硅纳米线的合成方法. 陈静.淮阴工学院学报，第15卷第3期. 2006 * |
| 碳化硅纳米管的制备和表征. 陶德良等.无机化学学报，第22卷第5期. 2006 |
| 碳化硅纳米管的制备和表征. 陶德良等.无机化学学报，第22卷第5期. 2006 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1962433A (en) | 2007-05-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kumar et al. | Sol-gel derived nanomaterials and it’s applications: a review | |
| CN106747530B (en) | Boron nitride nanosheet reinforced ceramic matrix composite and preparation method thereof | |
| CN106977221B (en) | A kind of SiCw-ZrB2- ZrC ceramic composite powder and preparation method thereof | |
| CN101935208B (en) | Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof | |
| CN100467374C (en) | Silicon carbide nano line containing associated noncrystalline sphere structure and its preparation method | |
| CN106006644A (en) | Preparation method of nano boron carbide powder | |
| CN101104515A (en) | SiC nano-wire and preparing method thereof | |
| CN109437203B (en) | Preparation method of high-purity one-dimensional SiC nano material | |
| CN113816379B (en) | Preparation method of nano hafnium boride powder | |
| CN110467467A (en) | A kind of bulky silicon carbide polymer precursor is ceramic and blending cracks preparation method again | |
| CN106192371B (en) | A kind of high temperature resistant 3Al2O3-2SiO2The preparation method of-SiBNC carbon fiber composite coatings | |
| CN110078521A (en) | A kind of submicron order silicon nitride hollow microsphere and preparation method | |
| Cao et al. | Preparation of zirconium diboride ultrafine hollow spheres by a combined sol–gel and boro/carbothermal reduction technique | |
| CN102701207B (en) | Method for preparing Al-doped silicon carbide nanowires | |
| CN110668447B (en) | Synthesis method of silicon carbide nanowire | |
| CN102351182A (en) | Preparation method of ultra-long silicon carbide nano-wires | |
| CN107602154A (en) | A kind of string-of-pearls-like SiC/SiO2Heterojunction structure and its synthetic method | |
| CN112030544B (en) | Method for in-situ growth of silicon carbide nanowires on surface of silicon carbide fiber | |
| CN113773090A (en) | ZrB2Preparation method of-ZrC-SiC nano composite ceramic material | |
| CN104973624B (en) | Preparation method of meshy tetragonal phase zirconia nano powder | |
| CN100445206C (en) | Method for preparing Nano composite material of amorphous carbon / silicon dioxide | |
| CN107473749A (en) | A kind of mullite complex phase fiber and preparation method thereof | |
| CN113735593B (en) | SiC with adjustable microstructure nws -ZrB 2 -ZrC hybrid ceramic powder and preparation method thereof | |
| CN110642261B (en) | Method for preparing sandwich type hollow sphere of boron phosphate loaded boron oxide compound through self-assembly template-free method | |
| CN111377735A (en) | Surface-modified nano zirconia ceramic powder and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090311 Termination date: 20100106 |