CN106629734A - Preparation method of silicon carbide nano material - Google Patents
Preparation method of silicon carbide nano material Download PDFInfo
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- CN106629734A CN106629734A CN201611200617.3A CN201611200617A CN106629734A CN 106629734 A CN106629734 A CN 106629734A CN 201611200617 A CN201611200617 A CN 201611200617A CN 106629734 A CN106629734 A CN 106629734A
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- resorcinol
- formaldehyde
- silicon dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention belongs to the field of silicon carbide nano materials, and particularly relates to a preparation method of a silicon carbide nano material. The method comprises the following steps: mixing resorcinol, formaldehyde, deionized water and sodium carbonate according to a certain mole ratio to obtain a resorcinol-formaldehyde sol; mixing ethyl orthosilicate, ethanol, deionized water and hydrochloric acid according to a certain mole ratio to obtain a silicon dioxide sol; mixing the resorcinol-formaldehyde sol and the silicon dioxide sol according to a certain mass ratio to obtain a resorcinol-formaldehyde/silicon dioxide composite aerogel; grinding the resorcinol-formaldehyde/silicon dioxide composite aerogel and iron nitrate to obtain an unpurified sample; and removing carbon and silicon dioxide from the unpurified sample to obtain the beta-silicon carbide nano material. The technical scheme solves the problems of difficulty in uniformly mixing the carbon source and silicon source, lower raw material utilization ratio, lower yield and the like in the silicon carbide nano material preparation process.
Description
Technical field
The invention belongs to silicon carbide nano material field, more particularly to a kind of preparation method of silicon carbide nano material.
Background technology
First generation elemental semiconductor with silicon as representative and the second generation compound semiconductor with GaAs representative are significantly
The development of microelectric technique and photoelectron technology has been promoted, but due to the restriction of material performance itself, its device application also becomes
In the limit.Compare with conventional semiconductor materials such as silicon and GaAs, carborundum possesses many excellent characteristics, such as band gap width,
Thermal conductivity is high, and critical breakdown electric field is high, and electronics saturation migration rate is high, and anti-oxidant anticorrosive heat-resisting ability is strong etc..Therefore with
Carborundum is that the third generation semiconductor of representative has been a great deal of attention, carborundum prepare high temperature, high frequency, it is high-power,
The aspect such as photoelectron and radioresistance device has huge potentiality.
In prior art, the preparation method of silicon carbide nano material mainly uses different carbon source, the carbon thermal reduction of silicon source
Method.During silicon carbide nano material is prepared, there is carbon source and silicon source is difficult to be well mixed, raw material availability is low, yield
Not high the problems such as.
The content of the invention
The embodiment of the present invention provides a kind of preparation method of silicon carbide nano material, solves and is preparing nanometer silicon carbide material
During material, the problems such as carbon source and silicon source are difficult to be well mixed, raw material availability is low, yield is not high, with process is simple, life
Produce low temperature, environmentally safe, power consumption is low, be easy to large-scale production, product purity height, good crystallinity, the skill of even thickness
Art effect.
The embodiment of the present invention provides a kind of preparation method of silicon carbide nano material, and methods described includes：According to mol ratio
1:2:10:0.01 amount weighs resorcinol, formaldehyde, deionized water and sodium carbonate, obtains resorcinol-first after stirring
Aldehyde colloidal sol；According to mol ratio 1:4:1:7.8×10-4Amount by tetraethyl orthosilicate, ethanol, deionized water and mixed in hydrochloric acid it is uniform after
Obtain silicon dioxide gel；By the resorcinol-formaldehyde colloidal sol and the silicon dioxide gel according to resorcinol and positive silicon
The mass ratio of acetoacetic ester is 1：Resorcinol-formaldehyde/silicon dioxide composite aerogel is obtained after 2.1 amount mixing and stirring；
Mol ratio according to carbon and slaine is 40～70 by the resorcinol-formaldehyde/silicon dioxide composite aerogel powder
It is ground with ferric nitrate, obtains unpurified sample；It is 3 with volume ratio after by the unpurified sample carbon elimination：1 hydrogen fluorine
Acid and red fuming nitric acid (RFNA) mixed liquor are processed and remove silica, and silicon B-carbide nano material is obtained.
Further, methods described also includes：According to mol ratio 1:4:1:7.8×10-4Amount by tetraethyl orthosilicate, second
After alcohol, deionized water and mixed in hydrochloric acid are uniform, stir 2 hours at 40 DEG C, room temperature is subsequently cooled to, according still further to certain ratio
Add the ammoniacal liquor and deionized water of 1mol/L so that the mol ratio of tetraethyl orthosilicate, ammoniacal liquor and this portions of de-ionized water is 1:5.7
×10-3:3, then be stirred at room temperature 10 minutes, obtain silicon dioxide gel.
Further, methods described also includes：By the resorcinol-formaldehyde colloidal sol and the silicon dioxide gel according to
The mass ratio of resorcinol and tetraethyl orthosilicate is 1：Inject after 2.1 amount mixing and stirring in ampoule bottle, sealing, at 85 DEG C
React 3 days in water-bath, form the transparent wet gel of dark red, the wet gel is dried 120 minutes in overcritical petroleum ether,
Prepared resorcinol-formaldehyde/silicon dioxide composite aerogel.
Further, methods described also includes：Mol ratio according to carbon and slaine is 40～70 by the isophthalic
Diphenol-formaldehyde/silicon dioxide composite aerogel powder is ground with ferric nitrate, and the mixture obtained after grinding is placed in into oxidation
In aluminium crucible, horizontal sliding enters in vacuum tube furnace, sealing, pump furnace air and be filled with argon gas, keep argon gas flow be 200～
300ml/min, is heat-treated according to the ramp of 5 DEG C/min to 1300 DEG C～1500 DEG C, is incubated 1～5 hour, is obtained not
Purification sample.
Further, methods described also includes：By the unpurified sample in 600 DEG C of air atmospheres calcination 5 hours with
Except carbon elimination.
Further, methods described also includes：It is 3 with volume ratio after by the unpurified sample carbon elimination：1 hydrogen fluorine
Acid and red fuming nitric acid (RFNA) mixed liquor are processed 72 hours, remove silica, then through deionized water cleaning and centrifugal treating, are dried, system
Obtain silicon B-carbide nano material.
Said one or multiple technical schemes in the embodiment of the present application, at least imitates with following one or more technology
Really：
In embodiments of the present invention, resorcinol-formaldehyde colloidal sol is obtained first, then silicon dioxide gel is obtained, by molten
Glue-gel technique, obtains resorcinol-formaldehyde/silicon dioxide composite aerogel that carbon element silicon is evenly distributed, this aeroge
Carbon element silicon and catalyst can be made to be mixed on nanometer level, reactivity is high, process is simple, in course of reaction almost
The pernicious gas for not polluting environment is produced, and is solved during silicon carbide nano material is prepared, and carbon source and silicon source are difficult to mix
The problems such as uniform, raw material availability is low, yield is not high is closed, with process is simple, raw material availability is high, it is low, right to produce temperature
Environmental nonpollution, consume energy it is low, it is easy to mass produce, product purity height, good crystallinity, the technique effect of even thickness.
Specific embodiment
The embodiment of the present invention provides a kind of preparation method of silicon carbide nano material, solves and is preparing nanometer silicon carbide material
During material, there are problems that carbon source and silicon source are difficult to be well mixed, raw material availability is low, yield not, with technique letter
Single, low production temperature, environmentally safe, power consumption are low, it is easy to mass produce, product purity height, good crystallinity, even thickness
Technique effect.
In order to solve above-mentioned technical problem, the thinking that the present invention is provided is as follows：
According to mol ratio 1:2:10:0.01 amount weighs resorcinol, formaldehyde, deionized water and sodium carbonate, and stirring is equal
Resorcinol-formaldehyde colloidal sol is obtained after even；According to mol ratio 1:4:1:7.8×10-4Amount by tetraethyl orthosilicate, ethanol, go from
Sub- water and hydrochloric acid (0.1mol/L) obtain silicon dioxide gel after being well mixed；By the resorcinol-formaldehyde colloidal sol and described
Silicon dioxide gel is 1 according to the mass ratio of resorcinol and tetraethyl orthosilicate：Isophthalic is obtained after 2.1 amount mixing and stirring
Diphenol-formaldehyde/silicon dioxide composite aerogel；Mol ratio according to carbon and slaine is 40～70 by the isophthalic two
Phenol-formaldehyde/silicon dioxide composite aerogel powder is ground with ferric nitrate, obtains unpurified sample；Will be described unpurified
Sample carbon elimination after, with volume ratio be 3：1 hydrofluoric acid and red fuming nitric acid (RFNA) mixed liquor are processed and remove silica, and prepared silicon B-carbide is received
Rice material.Solve during silicon carbide nano material is prepared, carbon source and silicon source are difficult to be well mixed, and raw material availability is inclined
It is low, the problems such as yield is not high.
Embodiment 1
The formaldehyde of 6.606g resorcinols and 8.8ml 37% is weighed, is mixed, add 10.8ml deionized waters as solvent
Adjust concentration, add 0.0636g sodium carbonate, then using magnetic stirring apparatus stir 15 minutes, make resorcinol, formaldehyde and
Sodium carbonate is full and uniform to be dissolved in water, and forms resorcinol-formaldehyde colloidal sol.
26.9ml tetraethyl orthosilicates, 28.0ml ethanol and 2.2ml deionized waters are mixed, instills 0.1mol/L's
Hydrochloric acid (HCl) 0.96ml, stirs 2 hours at 40 DEG C, is hydrolyzed；After in the case where solution is cooled to room temperature, then add
The ammoniacal liquor and 6.48ml deionized waters of 0.69ml 1mol/L, after 10min is stirred at room temperature, forms silicon dioxide gel.
In mass ratio 1.0:2.1 weigh 4.55g resorcinol-formaldehydes colloidal sol and the mixing of 9.55g silicon dioxide gels, then
Stirring 10 minutes, forms faint yellow, homogeneous mixed sols.By in this mixing colloidal sol injection ampoule bottle, sealing is placed in 85 DEG C of water
72 hours in bath, the wet gel of transparent dark red is formed, take out wet gel.It is dried 120 minutes in overcritical petroleum ether, system
Obtain resorcinol-formaldehyde/silicon dioxide composite aerogel.
It is 1 according to mass ratio：0.167 weigh 1.000g resorcinol-formaldehydes/silicon dioxide composite aerogel powder and
(wherein C/Fe mol ratios are 50 to 0.167g ferric nitrates：1), it is fully ground, mixture is placed in alumina crucible, horizontal sliding enters very
In empty tube furnace, sealing pumps furnace air, is filled with argon gas, then rises to predetermined temperature with the heating rate of 5 DEG C/min,
Heat treatment 1 hour is carried out at 1300 DEG C.After the completion of heating schedule, stand body of heater and be cooled to room temperature, take out unpurified sample.
First in air atmosphere 600 DEG C of calcinations with except carbon elimination, then with the mixing of hydrofluoric acid (40%) and nitric acid (65%)
Liquid (volume ratio 3：1) process 72 hours, remove silica, eventually pass deionized water cleaning and centrifugal treating, be dried, be obtained
The nanometer silicon B-carbide of purification, diameter 100nm or so, yield (ratio of actual production and raw material weight) is 64.9%.
Embodiment 2
The formaldehyde of 6.606g resorcinols and 8.8ml 37% is weighed, is mixed, add 10.8ml deionized waters as solvent
Adjust concentration, add 0.0636g sodium carbonate, then using magnetic stirring apparatus stir 15 minutes, make resorcinol, formaldehyde and
Sodium carbonate is full and uniform to be dissolved in water, and forms resorcinol-formaldehyde colloidal sol.
26.9ml tetraethyl orthosilicates, 28.0ml ethanol and 2.2ml deionized waters are mixed, instills 0.1mol/L's
Hydrochloric acid (HCl) 0.96ml, stirs 2 hours at 40 DEG C, is hydrolyzed；After in the case where solution is cooled to room temperature, then add
The ammoniacal liquor and 6.48ml deionized waters of 0.69ml 1mol/L, after 10min is stirred at room temperature, forms silicon dioxide gel.
In mass ratio 1.0:2.1 weigh 4.55g resorcinol-formaldehydes colloidal sol and the mixing of 9.55g silicon dioxide gels, then
Stirring 10 minutes, forms faint yellow, homogeneous mixed sols.By in this mixing colloidal sol injection ampoule bottle, sealing is placed in 85 DEG C of water
72 hours in bath, the wet gel of transparent dark red is formed, take out wet gel.It is dried 120 minutes in overcritical petroleum ether, system
Obtain resorcinol-formaldehyde/silicon dioxide composite aerogel.
It is 1 according to mass ratio：0.167 weigh 1.000g resorcinol-formaldehydes/silicon dioxide composite aerogel powder and
(wherein C/Fe mol ratios are 50 to 0.167g ferric nitrates：1), it is fully ground, mixture is placed in alumina crucible, horizontal sliding enters very
In empty tube furnace, sealing pumps furnace air, is filled with argon gas, then rises to predetermined temperature with the heating rate of 5 DEG C/min,
Heat treatment 1 hour is carried out at 1400 DEG C.After the completion of heating schedule, stand body of heater and be cooled to room temperature, take out unpurified sample.
First in air atmosphere 600 DEG C of calcinations with except carbon elimination, then with the mixing of hydrofluoric acid (40%) and nitric acid (65%)
Liquid (volume ratio 3：1) process 72 hours, remove silica, eventually pass deionized water cleaning and centrifugal treating, be dried, be obtained
The nanometer silicon B-carbide of purification, diameter 140nm or so, yield (ratio of actual production and raw material weight) is 35.1%.
Embodiment 3
The formaldehyde of 6.606g resorcinols and 8.8ml 37% is weighed, is mixed, add 10.8ml deionized waters as solvent
Adjust concentration, add 0.0636g sodium carbonate, then using magnetic stirring apparatus stir 15 minutes, make resorcinol, formaldehyde and
Sodium carbonate is full and uniform to be dissolved in water, and forms resorcinol-formaldehyde colloidal sol.
26.9ml tetraethyl orthosilicates, 28.0ml ethanol and 2.2ml deionized waters are mixed, instills 0.1mol/L's
Hydrochloric acid (HCl) 0.96ml, stirs 2 hours at 40 DEG C, is hydrolyzed；After in the case where solution is cooled to room temperature, then add
The ammoniacal liquor and 6.48ml deionized waters of 0.69ml 1mol/L, after 10min is stirred at room temperature, forms silicon dioxide gel.
In mass ratio 1.0:2.1 weigh 4.55g resorcinol-formaldehydes colloidal sol and the mixing of 9.55g silicon dioxide gels, then
Stirring 10 minutes, forms faint yellow, homogeneous mixed sols.By in this mixing colloidal sol injection ampoule bottle, sealing is placed in 85 DEG C of water
72 hours in bath, the wet gel of transparent dark red is formed, take out wet gel.It is dried 120 minutes in overcritical petroleum ether, system
Obtain resorcinol-formaldehyde/silicon dioxide composite aerogel.
It is 1 according to mass ratio：0.167 weigh 1.000g resorcinol-formaldehydes/silicon dioxide composite aerogel powder and
(wherein C/Fe mol ratios are 50 to 0.167g ferric nitrates：1), it is fully ground, mixture is placed in alumina crucible, horizontal sliding enters very
In empty tube furnace, sealing pumps furnace air, is filled with argon gas, then rises to predetermined temperature with the heating rate of 5 DEG C/min,
Heat treatment 2 hours is carried out at 1300 DEG C.After the completion of heating schedule, stand body of heater and be cooled to room temperature, take out unpurified sample.
First in air atmosphere 600 DEG C of calcinations with except carbon elimination, then with the mixing of hydrofluoric acid (40%) and nitric acid (65%)
Liquid (volume ratio 3：1) process 72 hours, remove silica, eventually pass deionized water cleaning and centrifugal treating, be dried, be obtained
The nanometer silicon B-carbide of purification, diameter 140nm or so, yield (ratio of actual production and raw material weight) is 59.4%.
A kind of preparation method of silicon carbide nano material that the embodiment of the present application of the present invention is provided has the following technical effect that：
In embodiments of the present invention, resorcinol-formaldehyde colloidal sol is obtained first, then silicon dioxide gel is obtained, by molten
Glue-gel technique, obtains resorcinol-formaldehyde/silicon dioxide composite aerogel that carbon element silicon is evenly distributed, this aeroge
Carbon element silicon and catalyst can be made to be mixed on nanometer level, reactivity is high, process is simple, in course of reaction almost
The pernicious gas for not polluting environment is produced, and is solved during silicon carbide nano material is prepared, and carbon source and silicon source are difficult to mix
The problems such as uniform, raw material availability is low, yield is not high is closed, with process is simple, raw material availability is high, it is low, right to produce temperature
Environmental nonpollution, consume energy it is low, be easy to large-scale production, product purity height, good crystallinity, the technique effect of even thickness.
, but those skilled in the art once know basic creation although preferred embodiments of the present invention have been described
Property concept, then can make other change and modification to these embodiments.So, claims are intended to be construed to include excellent
Select embodiment and fall into having altered and changing for the scope of the invention.
Obviously, those skilled in the art can carry out the essence of various changes and modification without deviating from the present invention to the present invention
God and scope.So, if these modifications of the present invention and modification belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising these changes and modification.
Claims (6)
1. a kind of preparation method of silicon carbide nano material, it is characterised in that methods described includes：
According to mol ratio 1:2:10:0.01 amount weighs resorcinol, formaldehyde, deionized water and sodium carbonate, after stirring
Obtain resorcinol-formaldehyde colloidal sol；
According to mol ratio 1:4:1:7.8×10-4Amount tetraethyl orthosilicate, ethanol, deionized water and hydrochloric acid (0.1mol/L) is mixed
Silicon dioxide gel is obtained after closing uniformly；
By the resorcinol-formaldehyde colloidal sol and the silicon dioxide gel according to resorcinol and the mass ratio of tetraethyl orthosilicate
For 1：Resorcinol-formaldehyde/silicon dioxide composite aerogel is obtained after 2.1 amount mixing and stirring；
Mol ratio according to carbon and slaine is 40～70 by the resorcinol-formaldehyde/silicon dioxide composite aerogel
Powder is ground with ferric nitrate, obtains unpurified sample；
It is 3 with volume ratio after by the unpurified sample carbon elimination：1 hydrofluoric acid and red fuming nitric acid (RFNA) mixed liquor are processed and remove dioxy
SiClx, is obtained silicon B-carbide nano material.
2. the method for claim 1, it is characterised in that methods described also includes：
According to mol ratio 1:4:1:7.8×10-4Amount by tetraethyl orthosilicate, ethanol, deionized water and mixed in hydrochloric acid it is uniform after,
Stir 2 hours at 40 DEG C, be subsequently cooled to room temperature, according still further to certain ratio the ammoniacal liquor and deionized water of 1mol/L are added, make
The mol ratio for obtaining tetraethyl orthosilicate, ammoniacal liquor and this portions of de-ionized water is 1:5.7×10-3:3, then be stirred at room temperature 10 minutes,
Obtain silicon dioxide gel.
3. the method for claim 1, it is characterised in that methods described also includes：
By the resorcinol-formaldehyde colloidal sol and the silicon dioxide gel according to resorcinol and the mass ratio of tetraethyl orthosilicate
For 1：Inject after 2.1 amount mixing and stirring in ampoule bottle, sealing is reacted 3 days in 85 DEG C of water-baths, forms the saturating of dark red
Bright wet gel, the wet gel is dried 120 minutes in overcritical petroleum ether, resorcinol-formaldehyde/silica is obtained multiple
Close aeroge.
4. the method for claim 1, it is characterised in that methods described also includes：
Mol ratio according to carbon and slaine is 40～70 by the resorcinol-formaldehyde/silicon dioxide composite aerogel
Powder is ground with ferric nitrate, and the mixture obtained after grinding is placed in alumina crucible, and horizontal sliding enters in vacuum tube furnace,
Sealing, pumps furnace air and is filled with argon gas, and the flow for keeping argon gas is 200～300ml/min, according to the speed of 5 DEG C/min
It is warming up to 1300 DEG C～1500 DEG C to be heat-treated, is incubated 1～5 hour, obtains unpurified sample.
5. the method for claim 1, it is characterised in that methods described also includes：
By the unpurified sample in 600 DEG C of air atmospheres calcination 5 hours with except carbon elimination.
6. the method for claim 1, it is characterised in that methods described also includes：
It is 3 with volume ratio after by the unpurified sample carbon elimination：1 hydrofluoric acid and red fuming nitric acid (RFNA) mixed liquor are processed 72 hours, are removed
Silica is removed, then through deionized water cleaning and centrifugal treating, is dried, silicon B-carbide nano material is obtained.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186297A (en) * | 2007-12-21 | 2008-05-28 | 中国科学院山西煤炭化学研究所 | Method for preparing silicon carbide nano-wire with periodical twin crystal structure |
| CN104907016A (en) * | 2014-03-11 | 2015-09-16 | 北京化工大学 | Preparation method of carbon aerogel |
| CN105000562A (en) * | 2015-07-31 | 2015-10-28 | 中国计量学院 | Preparation method of silicon carbide hollow sphere |
-
2016
- 2016-12-22 CN CN201611200617.3A patent/CN106629734A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186297A (en) * | 2007-12-21 | 2008-05-28 | 中国科学院山西煤炭化学研究所 | Method for preparing silicon carbide nano-wire with periodical twin crystal structure |
| CN104907016A (en) * | 2014-03-11 | 2015-09-16 | 北京化工大学 | Preparation method of carbon aerogel |
| CN105000562A (en) * | 2015-07-31 | 2015-10-28 | 中国计量学院 | Preparation method of silicon carbide hollow sphere |
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| 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Application publication date: 20170510 |