CN101864619A - Method for preparing nanometer-diameter carborundum brief fiber and whisker by utilizing rice hulls - Google Patents
Method for preparing nanometer-diameter carborundum brief fiber and whisker by utilizing rice hulls Download PDFInfo
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- CN101864619A CN101864619A CN 201010202371 CN201010202371A CN101864619A CN 101864619 A CN101864619 A CN 101864619A CN 201010202371 CN201010202371 CN 201010202371 CN 201010202371 A CN201010202371 A CN 201010202371A CN 101864619 A CN101864619 A CN 101864619A
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- whisker
- rice husk
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- rice hulls
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Abstract
The invention relates to a method for preparing nanometer-diameter carborundum brief fiber and whisker by utilizing rice hulls. In a graphite crucible, cleaned and dried rice hulls are added and carbonized at certain temperature in a vacuum furnace; the carbonized rice hulls and one or two catalysts are evenly and mechanically mixed, or the catalyst is not added; the rice hulls which are evenly mixed and catalyzed or the rice hulls which are carbonized without adding catalyst are added into the graphite crucible, a graphite cover is covered on the graphite crucible, and the graphite crucible is placed into a vacuum sintering furnace; inert gas is introduced in for protection, and temperature rises at a certain rate and subsequently lowers to room temperature; the sintering furnace is opened, the upper surface of the rice hulls in the graphite crucible is provided with white flocculent carborundum brief fiber and whisker; and white to baby blue flocculent carborundum brief fiber and whisker are generated among the rice hulls. The carborundum brief fiber and the whisker prepared by the invention have high purity and high length-diameter ratio, the diameter of the whisker is 10-200 nanometers, and the length of the whisker is up to 8mm. The invention has low production cost, simple production process and simple production equipment.
Description
Technical field:
The present invention relates to a kind of preparation method of carborundum, especially utilize biological material to prepare the method for carborundum brief fiber and whisker.
Background technology:
In recent years, the one-dimensional micro-nanometer material because its special physics that has, chemical property and in opto-electronic device huge potential application foreground, caused that people are to the preparation of one-dimensional micro-nanometer material and the very big interest of performance study.And SiC staple fibre and whisker have high chemical stability, the specific strength height, the specific stiffness height, resistance to high temperature oxidation, can good chemical intermiscibility and bond strength be arranged with metals such as aluminium, magnesium, titanium and oxides such as aluminium oxide, zirconia, be the good reinforcing material of Metal Substrate and ceramic matric composite.Fields such as machinery, electronics, chemical industry, the energy, Aero-Space and environmental protection have been widely used in.Simultaneously, SiC staple fibre and whisker have high energy gap, high critical breakdown electric field and thermal conductivity, and little dielectric constant and the saturated mobility of higher electronics become the ideal material of making nano photoelectronic devices.The method for preparing at present SiC staple fibre and whisker can be divided into two kinds: a kind of is gas-phase reaction method, contains the organic gas of carbon, silicon compound with carbonaceous gas and silicon-containing gas reaction or decomposition.Another kind of for the solid material utilization contains the composite material of carbon and silicon, at material gap formation SiC staple fibre and whisker.The reaction mechanism that SiC staple fibre and whisker form mainly contains: synthetic and synthetic SiC staple fibre of VS (steam-solid phase) and whisker by VLS (steam-liquid-solid phase).The concrete method that prepare SiC staple fibre and whisker has: with rice husk synthesize, organo-silicon compound pyrolysis, silicon halide and CCl
4Deng mixed gas reaction, oxide containing silicon carbon thermal reduction etc.The problem that the SiC whisker for preparing in order to the top method exists has: environmental pollution, preparation equipment require height, complicated process of preparation etc.
Summary of the invention:
Purpose of the present invention is exactly at above-mentioned the deficiencies in the prior art, and a kind of method of utilizing rice husk to prepare nanometer-diameter carborundum brief fiber and whisker is provided.
The objective of the invention is to be achieved through the following technical solutions:
Utilize rice husk to prepare the method for nanometer-diameter carborundum brief fiber and whisker, comprise following order and step:
A, in graphite crucible, add the rice husk behind the cleaning-drying, in vacuum drying oven under 460-700 ℃ of temperature carbonization 1-2 hour;
B, the rice husk after the carbonization and one or both catalyst mechanical mixture is even, or do not add catalyst;
C, the rice husk after mixing the rice husk after the catalysis or not adding the catalyst carbonization is put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 5-20Pa, feed inert gas, make furnace pressure be controlled at .01-0.05MPa, close gas valve, be heated to 1300-1450 ℃, be incubated 1-4 hour with 20-30 ℃ of/minute heating rate, powered-down is with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
Purpose of the present invention can also be achieved through the following technical solutions:
The described catalyst of step b is that micron order Fe powder or NaF analysis are pure.Catalyst addition by weight percentage is 0-10%wt.
Beneficial effect: use the carborundum brief fiber and the whisker purity height of the present invention's preparation, carborundum brief fiber and whisker draw ratio are big, diameter of whiskers 10-200 nanometer, and length can arrive 8mm, and production cost is low, and production technology is simple, and production equipment is simple.
Description of drawings:
Accompanying drawing 1 carborundum brief fiber and whisker (SEM) photo
Accompanying drawing 2 fibers and whisker (TEM) photo
The specific embodiment:
Be described in further detail below in conjunction with drawings and Examples:
Utilize rice husk to prepare the method for nanometer-diameter carborundum brief fiber and whisker, comprise following order and step:
A, in graphite crucible, add the rice husk behind the cleaning-drying, in vacuum drying oven under 460-700 ℃ of temperature carbonization 1-2 hour;
B, the rice husk after the carbonization and one or both catalyst mechanical mixture is even, or do not add catalyst;
C, the rice husk after mixing the rice husk after the catalysis or not adding the catalyst carbonization is put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 5-20Pa, feed inert gas, make furnace pressure be controlled at 0.01-0.05MPa, close gas valve, be heated to 1300-1450 ℃, be incubated 1-4 hour with 20-30 ℃ of/minute heating rate, powered-down is with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
The described catalyst of step b is that micron order Fe powder or NaF analysis are pure.Catalyst addition by weight percentage is 0-10%wt.
Embodiment 1
A, the rice husk of getting behind the 300g cleaning-drying place crucible, carbonization 2 hours under 460 ℃ of temperature in vacuum drying oven;
B, that the rice husk 93.2g after the carbonization and micron order Fe powder 2.6g and NaF are analyzed pure 4.2g mechanical mixture is even;
C, the rice husk that will mix behind the catalyst are put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 10Pa, feed argon shield, make furnace pressure be controlled at 0.03MPa, stop to feed argon gas, be heated to 1400 ℃, be incubated 2 hours with 30 ℃ of/minute heating rates, powered-down is with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.See accompanying drawing 1
Embodiment 2
A, the rice husk of getting behind the 300g cleaning-drying place crucible, carbonization 1.5 hours under 500 ℃ of temperature in vacuum drying oven;
B, that the rice husk 92.5g after the carbonization and micron order Fe powder 5g and NaF are analyzed pure 2.5g mechanical mixture is even;
C, the rice husk that will mix behind the catalyst are put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 5Pa, feed nitrogen protection, furnace pressure is controlled at 0.05MPa, stop to feed, be heated to 1400 ℃, be incubated 3 hours with 20 ℃ of/minute heating rates, powered-down is with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
Embodiment 3
A, the rice husk of getting behind the 300g cleaning-drying place crucible, carbonization 1 hour under 550 ℃ of temperature in vacuum drying oven;
B, that the rice husk 93g after the carbonization and micron order Fe powder 5g and NaF are analyzed pure 2g mechanical mixture is even;
C, the rice husk that will mix behind the catalyst are put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 20Pa, feed argon shield, furnace pressure is controlled at 0.04MPa, stop to feed argon gas, be heated to 1450 ℃, be incubated 1 hour with 25 ℃ of/minute heating rates, powered-down is with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
Embodiment 4
A, the rice husk of getting behind the 300g cleaning-drying place crucible, carbonization 1 hour under 600 ℃ of temperature in vacuum drying oven;
B, with rice husk 95g after the carbonization and micron order Fe powder 5g, mechanical mixture is even;
C, the rice husk that will mix behind the catalyst are put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 10Pa, feed argon shield, furnace pressure is controlled at 0.03MPa, stop to feed argon gas, be heated to 1300 ℃, be incubated 3 hours with 20 ℃ of/minute heating rates, powered-down is with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
Embodiment 5
A, the rice husk of getting behind the 300g cleaning-drying place crucible, carbonization 1 hour under 600 ℃ of temperature in vacuum drying oven;
B, the rice husk after the carbonization is put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 10Pa, feed argon shield, furnace pressure is controlled to be 0.02MPa, stop to feed argon gas, be heated to 1400 ℃ with 30 ℃ of/minute heating rates, be incubated 4 hours powered-downs, with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
Embodiment 6
A, the rice husk of getting behind the 300g cleaning-drying place crucible, carbonization 1 hour under 700 ℃ of temperature in vacuum drying oven;
B, that the rice husk 95g after the carbonization and NaF are analyzed pure 5g mechanical mixture is even;
C, the rice husk that will mix behind the catalyst are put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 5Pa, feed argon shield, furnace pressure is controlled to be 0.01MPa, stop to feed argon gas, be heated to 1400 ℃, be incubated 3 hours with 30 ℃ of/minute heating rates, powered-down is with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
Claims (4)
1. method of utilizing rice husk to prepare nanometer-diameter carborundum brief fiber and whisker is characterized in that: comprise following order and step:
A, in graphite crucible, add the rice husk behind the cleaning-drying, in vacuum drying oven under 460-700 ℃ of temperature carbonization 1-2 hour;
B, the rice husk after the carbonization and one or both catalyst mechanical mixture is even, or do not add catalyst;
C, the rice husk after mixing the rice husk after the catalysis or not adding the catalyst carbonization is put into graphite crucible, cover graphite cover, put into vacuum sintering furnace, be evacuated to 5-20Pa, feed inert gas, make furnace pressure be controlled at 0.01-0.05MPa, close gas valve, be heated to 1300-1450 ℃, be incubated 1-4 hour with 20-30 ℃ of/minute heating rate, powered-down is with the stove cool to room temperature;
D, open sintering furnace, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the graphite crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
2. according to the described method of utilizing rice husk to prepare nanometer-diameter carborundum brief fiber and whisker of claim 1, it is characterized in that: the described catalyst of step b is that micron order Fe powder or NaF analysis are pure.
3. according to the described method of utilizing rice husk to prepare nanometer-diameter carborundum brief fiber and whisker of claim 1, it is characterized in that: the described inert gas of step c is argon gas or nitrogen.
4. according to the described method of utilizing rice husk to prepare nanometer-diameter carborundum brief fiber and whisker of claim 2, it is characterized in that: catalyst addition by weight percentage is 0-10%wt.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161594A (en) * | 2011-05-12 | 2011-08-24 | 浙江大学 | SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof |
| CN102219536A (en) * | 2011-04-27 | 2011-10-19 | 浙江大学 | B4C/SiC whisker/SiC multiphase ceramic matrix composite and preparation method thereof |
| CN103382030A (en) * | 2012-05-04 | 2013-11-06 | 江苏瑞力新材料科技有限公司 | Preparation method and use of nano-SiC whisker |
| CN103803982A (en) * | 2014-02-27 | 2014-05-21 | 中原工学院 | Preparation method of rice hull stacked porous silicon carbide |
| CN106282927A (en) * | 2016-08-05 | 2017-01-04 | 宁波高新区斯汀环保科技有限公司 | A kind of preparation method of molybdenum carbon modified SiClx/copper composite electron encapsulating material |
| CN106800420A (en) * | 2016-12-30 | 2017-06-06 | 河南工业大学 | A kind of silicon carbide whisker in-situ composite corindon high-temperature ceramic materials and preparation method thereof |
| CN108486401A (en) * | 2018-05-25 | 2018-09-04 | 北汽新能源汽车常州有限公司 | Al-alloy, preparation method and application |
| CN116856066A (en) * | 2023-09-01 | 2023-10-10 | 宁波合盛新材料有限公司 | Silicon carbide seed crystal bonding method |
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| JPS57209813A (en) * | 1981-06-18 | 1982-12-23 | Tokai Carbon Co Ltd | Preparation of silicon carbide whisker |
| CN1087332A (en) * | 1992-11-27 | 1994-06-01 | 中南工业大学 | Produce graphite coat of silicon carbide and carbon-silicon compound with rice hulls |
| CN1385558A (en) * | 2002-03-01 | 2002-12-18 | 徐宏武 | Preparation of nano grade Sic/SiO2 by high silicon coal and whisker/fibre thereof |
| CN1721583A (en) * | 2005-05-24 | 2006-01-18 | 西北工业大学 | Process for preparing silicon carbide crystal whisker |
| CN1803599A (en) * | 2005-05-31 | 2006-07-19 | 株洲工学院科技开发部 | Process and apparatus for preparing high-purity silicon dioxide by utilizing rice hull |
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2010
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57209813A (en) * | 1981-06-18 | 1982-12-23 | Tokai Carbon Co Ltd | Preparation of silicon carbide whisker |
| CN1087332A (en) * | 1992-11-27 | 1994-06-01 | 中南工业大学 | Produce graphite coat of silicon carbide and carbon-silicon compound with rice hulls |
| CN1385558A (en) * | 2002-03-01 | 2002-12-18 | 徐宏武 | Preparation of nano grade Sic/SiO2 by high silicon coal and whisker/fibre thereof |
| CN1721583A (en) * | 2005-05-24 | 2006-01-18 | 西北工业大学 | Process for preparing silicon carbide crystal whisker |
| CN1803599A (en) * | 2005-05-31 | 2006-07-19 | 株洲工学院科技开发部 | Process and apparatus for preparing high-purity silicon dioxide by utilizing rice hull |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219536A (en) * | 2011-04-27 | 2011-10-19 | 浙江大学 | B4C/SiC whisker/SiC multiphase ceramic matrix composite and preparation method thereof |
| CN102161594A (en) * | 2011-05-12 | 2011-08-24 | 浙江大学 | SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof |
| CN102161594B (en) * | 2011-05-12 | 2013-02-06 | 浙江大学 | SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof |
| CN103382030A (en) * | 2012-05-04 | 2013-11-06 | 江苏瑞力新材料科技有限公司 | Preparation method and use of nano-SiC whisker |
| CN103803982A (en) * | 2014-02-27 | 2014-05-21 | 中原工学院 | Preparation method of rice hull stacked porous silicon carbide |
| CN103803982B (en) * | 2014-02-27 | 2016-02-17 | 中原工学院 | Rice husk piles up the preparation method of porous silicon carbide |
| CN106282927A (en) * | 2016-08-05 | 2017-01-04 | 宁波高新区斯汀环保科技有限公司 | A kind of preparation method of molybdenum carbon modified SiClx/copper composite electron encapsulating material |
| CN106800420A (en) * | 2016-12-30 | 2017-06-06 | 河南工业大学 | A kind of silicon carbide whisker in-situ composite corindon high-temperature ceramic materials and preparation method thereof |
| CN108486401A (en) * | 2018-05-25 | 2018-09-04 | 北汽新能源汽车常州有限公司 | Al-alloy, preparation method and application |
| CN116856066A (en) * | 2023-09-01 | 2023-10-10 | 宁波合盛新材料有限公司 | Silicon carbide seed crystal bonding method |
| CN116856066B (en) * | 2023-09-01 | 2023-11-14 | 宁波合盛新材料有限公司 | Silicon carbide seed crystal bonding method |
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Application publication date: 20101020 |