CN107963631A - Nanometer silicon carbide and preparation method thereof - Google Patents
Nanometer silicon carbide and preparation method thereof Download PDFInfo
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- CN107963631A CN107963631A CN201711321349.5A CN201711321349A CN107963631A CN 107963631 A CN107963631 A CN 107963631A CN 201711321349 A CN201711321349 A CN 201711321349A CN 107963631 A CN107963631 A CN 107963631A
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Abstract
The invention belongs to a kind of inorganic compound field of nanometer material technology, more particularly to a kind of nanometer silicon carbide and preparation method thereof, the nanometer silicon carbide pore-size distribution is 16 48nm, and the nanometer silicon carbide particle diameter is 8 16nm, and the specific surface area of the nanometer silicon carbide is 120 180m2/ g, there is the pore structure of multidimensional hydridization between the particle of the nanometer silicon carbide, in addition the present invention also provides a kind of preparation method of above-mentioned nanometer silicon carbide, technical solution using the present invention has the advantages that simple to equipment requirement, process is easily operated, production life cycle is short, and the method for preparing nanometer silicon carbide cost-effective can obtain the required nanometer silicon carbide in this area.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic compound nano material, a kind of nano silicon carbide has been related in particular to
Silicon and preparation method thereof.
Technical background
Nm-class silicon carbide material has high energy gap, high critical breakdown electric field and thermal conductivity, small dielectric constant
Higher electronics saturation mobility, and capability of resistance to radiation are strong, the characteristic such as good mechanical property, become make high frequency, it is high-power,
The ideal material of low energy consumption, the electronics of high temperature resistant and radioresistance device and opto-electronic device, is generally considered to be expected to become the 3rd
For the important composition unit of wide bandgap semiconductor materials.
The preparation method for preparing nanometer silicon carbide at present has ball-milling method, plasma method and carbothermic method.Above method ball
Mill method process is more complicated, high energy consumption, and plasma method needs the expensive and poisonous silicon precursor that contains, and carbon thermal reduction needs
Nano level presoma is as raw material and reaction temperature is more than 1400 DEG C, such as a kind of patent " preparation side of β-nanometer silicon carbide
Method " (CN102432013B) is so as to limit its low cost and large-scale application.
Become the only way which must be passed of its large-scale application using cheap raw material low temperature preparation nanometer silicon carbide, in recent years,
Use siliceous discarded object for raw material to prepare nanometer silicon carbide and cause widely to pay close attention to.For example silicon containing biomass is used as original
Material, the nanometer silicon dioxide particle formed using biomineralization in biomass are prepared using magnesiothermic reduction method and received and paid out as predecessor
Rice nanometer silicon carbide particle.
In addition, porous nano carborundum is due to big specific surface area, so as to show the performance of uniqueness.The prior art is general
Porous silicon carbide (SiO is prepared using magnesiothermic reduction reaction using porous silica nanometer structure as predecessor2+ C+2Mg=
SiC+2MgO), the pattern of reaction product heredity predecessor silica, but predecessor silica is of high cost in this method,
Structure is easily caved in.And product is generally nano particle obtained by using the predecessors such as biomass as raw material, it is difficult to obtain porous
Nanometer silicon carbide.
The content of the invention
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of nanometer silicon carbide and its preparation side
Method, the nanometer silicon carbide pore-size distribution are 16-48nm, and the nanometer silicon carbide particle diameter is 8-16nm, the nanometer silicon carbide
Specific surface area be 120-180m2/ g, has the pore structure of multidimensional hydridization between the particle of the nanometer silicon carbide.
In a preferable scheme, the specific nanometer silicon carbide pore-size distribution can be 16nm, 20nm, 24nm,
Arbitrary Digit in the scope that any two in 28nm, 32nm, 36nm, 40nm, 44nm, 48nm and these numerical value is formed
Value.
In a preferable scheme, the specific nanometer silicon carbide particle diameter can be 8nm, 9nm, 10nm, 11nm,
Any number in the scope that any two in 12nm, 13nm, 14nm, 15nm, 16nm and these numerical value is formed.
In a preferable scheme, the specific surface area of the specific nanometer silicon carbide can be 120m2/g、130m2/g、
140m2/g、150m2/g、160m2/g、170m2/g、180m2In the scope that any two in/g and these numerical value is formed
Any number.
Another aspect of the present invention also provides a kind of preparation method for preparing above-mentioned nanometer silicon carbide, and this method includes following step
Suddenly：
(1) solvent that 5-8 parts by weight are added in the surfactant of 1 parts by weight and the carbonate of 0.3-0.8 parts by weight is taken,
Then under conditions of stirring, the ethyl orthosilicate of 3-8 parts by weight and the catalyst of 0.1-0.3 parts by weight are added, at room temperature just
Silicate hydrolyzate 12-72h, forms SiO2Colloidal sol；
(2) in SiO2Colloidal sol adds the set agent of 0.2-0.5 parts by weight, forms SiO2Gel, then at 80 DEG C -180 DEG C
Dry 24-48h forms SiO2Xerogel, then by SiO2Xerogel is obtained more in 750 DEG C of -1000 DEG C of Muffle kiln roasting 4-12h
Hole SiO2；
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 1-5 mixing, CO is continuously passed through
Gas, 1350 DEG C -1500 DEG C are heated to the heating rate of 5-12 DEG C/min, and constant temperature 8-36h, is cooled to room temperature, are obtained initial
Product, then by initial product through peroxidating, acid soak, wash and be dried to obtain nanometer silicon carbide.
In a preferable scheme, the surfactant is phenolic resin, hexadecyltrimethylammonium chloride, 16
At least one of alkyl trimethyl ammonium bromide, polyethylene glycol, biphenyl, furfural, saccharide compound.Term " surface in the present invention
Activating agent " refers to add the material that can make the interface state of its solution system that significant change occur on a small quantity.With fixed hydrophilic
Lipophilic group, aligns in the surface energy of solution.The molecular structure of surfactant has amphipathic：One end is hydrophilic group
Group, the other end is hydrophobic grouping；Hydrophilic radical is often polar group, such as carboxylic acid, sulfonic acid, sulfuric acid, amino or amido and its salt, hydroxyl
Base, amide groups, ehter bond etc. can also be used as polar hydrophilic group；And hydrophobic grouping is often nonpolar hydrocarbon chain, more than 8 carbon atoms
Hydrocarbon chain.Surfactant be divided into ionic surfactant (including cationic surfactant and anion surfactant),
Nonionic surface active agent, amphoteric surfactant, compound surfactant, other surfaces activating agent etc..
In a preferable scheme, the saccharide compound is at least one of sucrose, fructose, fructose.
In a preferable scheme, the catalyst is oxalic acid, hydrochloric acid, nitric acid, hydrofluoric acid, sodium hydroxide, hydroxide
Potassium or ammonium hydroxide.
In a preferable scheme, the carbonate is sodium carbonate, potassium carbonate, sodium acid carbonate, in saleratus extremely
Few one kind, it is further preferred that the carbonate sodium acid carbonate and/or saleratus.
In a preferable scheme, the granularity of the graphite powder is 45-200 μm, the granularity of the specific graphite powder
Can be in 45 μm, 65 μm, 85 μm, 100 μm, 120 μm, 120 μm, 140 μm, 160 μm, 180 μm, 200 μm and these numerical value
Any number in the scope that any two is formed, the carbon content of the graphite powder is ＞ 99.5%.
In a preferable scheme, the set agent is hexamethylenetetramine, in resol, amino resins
At least one.Term " set agent " refers to a kind of material or mixture promoted or control curing reaction in the present invention.Resin
Curing is chemically reacted by condensation, closed loop, addition or catalysis etc., makes thermosetting resin that irreversible change procedure occur, Gu
Change is completed by adding curing (crosslinking) agent.Curing agent is essential additive, either makees bonding agent, applies
Material, castable all need addition curing agent, and otherwise epoxy resin cannot cure.The kind of curing agent to the mechanical property of solidfied material,
Heat resistance, water resistance, corrosion resistance etc. all have a significant impact.
In a preferable scheme, the condition of the oxidation is：Temperature is 600-900 DEG C, time 4-12h；It is described
The condition of acid soak is：Time is 24-120h；The condition of the washing is：Deionized water is washed 8-16 times；The drying
Condition is：Temperature is 110-220 DEG C, time 12-24h；
In a preferable scheme, the acid solution is that volume ratio is 1：The hydrochloric acid of 2-5 and the mixed acid of hydrofluoric acid, specifically
The hydrochloric acid and hydrofluoric acid volume ratio can be 1:2、1:3、1:4、1:5 and these numerical value in any two formed
Any number in scope.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show
Beneficial effect：Technical solution using the present invention has the advantages that simple to equipment requirement, process is easily operated, production life cycle is short,
And preparing the method for nanometer silicon carbide cost-effective can obtain the required nanometer silicon carbide in this area.
Brief description of the drawings
Fig. 1 is the XRD spectrum for the nano silicon carbide granulate that the embodiment of the present invention 1 is prepared；
Fig. 2 is adsorption and desorption curve and the aperture for the nano silicon carbide granulate that the embodiment of the present invention 1 is prepared
Distribution curve.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not forming conflict each other can be mutually combined.
Present embodiment discloses a kind of nanometer silicon carbide, the nanometer silicon carbide pore-size distribution is 16-48nm, the nanometer
Carborundum particle diameter is 8-16nm, and the specific surface area of the nanometer silicon carbide is 120-180m2/ g, the particle of the nanometer silicon carbide
Between have multidimensional hydridization pore structure.
On the other hand this is the invention also discloses a kind of preparation method for preparing above-mentioned nanometer silicon carbide, and this method is including such as
Lower step：
(1) solvent that 5-8 parts by weight are added in the surfactant of 1 parts by weight and the carbonate of 0.3-0.8 parts by weight is taken,
Then under conditions of stirring, the ethyl orthosilicate of 3-8 parts by weight and the catalyst of 0.1-0.3 parts by weight are added, at room temperature just
Silicate hydrolyzate 12-72h, forms SiO2Colloidal sol；
(2) in SiO2Colloidal sol adds the set agent of 0.2-0.5 parts by weight, forms SiO2Gel, then at 80 DEG C -180 DEG C
Dry 24-48h forms SiO2Xerogel, then by SiO2Xerogel is obtained more in 750 DEG C of -1000 DEG C of Muffle kiln roasting 4-12h
Hole SiO2；
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 1-5 mixing, CO is continuously passed through
Gas, 1350 DEG C -1500 DEG C are heated to the heating rate of 5-12 DEG C/min, and constant temperature 8-36h, is cooled to room temperature, are obtained initial
Product, then by initial product through peroxidating, acid soak, wash and be dried to obtain nanometer silicon carbide.
It is embodiment below：
Embodiment 1
(1) 12 grams of phenolic resin and 3.2 grams of sodium acid carbonates are weighed in beaker, add 60 milliliters of absolute ethyl alcohol, stirring
It is allowed to dissolve, under agitation, adds 36 milliliters of ethyl orthosilicates and 1.2 grams of oxalic acid, at room temperature teos hydrolysis
12h, forms SiO2Colloidal sol.
(2) in SiO2Colloidal sol adds 2.4 grams of curing agent hexamethylenetetramines, accelerates colloidal sol solidification, forms gel, Ran Hou
Dry 24h, obtains SiO under the conditions of 80 DEG C2Xerogel, then by SiO2Xerogel is accompanied in 750 DEG C of Muffle furnaces burns 4h, then removes
Template phenolic resin, obtains porous SiO2。
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 1 mixing, CO gas is continuously passed through
Body, 1350 DEG C are heated to the heating rate of 5 DEG C/min, and constant temperature 8h, is cooled to room temperature, obtain initial product, then will initially produce
Thing aoxidizes 4h in 600 DEG C of air, soaks 24h after cooling and then in the hydrochloric acid and the mixed acid of hydrofluoric acid that volume ratio is 1: 2,
Then use and washed in deionized water 8 times, 12h is finally dried in 110 DEG C of drying box.
It is embodiment 1 based on nanometer silicon carbide made from the present embodiment method.
Phenetic analysis is carried out to the porous nano silicon-carbide particle being prepared：
From the XRD diffracting spectrums of Fig. 1, three strongest peak and carborundum (JCPDSNo.29- at 35.6 °, 60 ° and 71.8 °
1129) three strongest peak is corresponding, and substantially without dephasign.
From the adsorption and desorption curve and pore size distribution curve of Fig. 2, the carborundum that the present embodiment is prepared
There is product excellent pore passage structure and overall structure not to destroy, and is connected with each other between nano silicon carbide granulate, nano silicon carbide
There is the hole of perforation, the nanometer silicon carbide pore-size distribution is 16-24nm, and the nanometer silicon carbide particle diameter is 8- between silicon grain
10nm, the specific surface area of the nanometer silicon carbide is 120-140m2/ g, the nanometer silicon carbide of the method synthesis have the ratio of superelevation
Surface area and excellent pore structure, therefore the porous nano carborundum of the present invention industrially can be mass produced and applied.
Embodiment 2
(1) 12 grams of phenolic resin and 4.8 grams of sodium acid carbonates are weighed in beaker, add 72 milliliters of absolute ethyl alcohol, stirring
It is allowed to dissolve, under agitation, adds 40 milliliters of ethyl orthosilicates and 3.6 grams of oxalic acid, at room temperature teos hydrolysis
24h, forms SiO2Colloidal sol.
(2) in SiO2Colloidal sol adds 2.8 grams of curing agent hexamethylenetetramines, accelerates colloidal sol solidification, forms gel, Ran Hou
Dry 30h, obtains SiO under the conditions of 100 DEG C2Xerogel, then by SiO2Xerogel is accompanied in 800 DEG C of Muffle furnaces burns 8h, then removes
Template phenolic resin, obtains porous SiO2。
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 2 mixing, CO gas is continuously passed through
Body, 1450 DEG C are heated to the heating rate of 6 DEG C/min, and constant temperature 10h, is cooled to room temperature, obtain initial product, then will initially produce
Thing aoxidizes 6h in 650 DEG C of air, soaks 36h after cooling and then in the hydrochloric acid and the mixed acid of hydrofluoric acid that volume ratio is 1: 3,
Then use and washed in deionized water 9 times, 12h is finally dried in 130 DEG C of drying box.
It is embodiment 2 based on nanometer silicon carbide made from the present embodiment method.
Phenetic analysis is carried out to the porous nano silicon-carbide particle being prepared：
From the XRD diffracting spectrums of embodiment 2, in 35.6 °, 60 ° and 71.8 ° of three strongest peak and carborundum
(JCPDSNo.29-1129) three strongest peak is corresponding, and substantially without dephasign.
Knowable to the adsorption and desorption curve and pore size distribution curve of embodiment 2, the carbonization that the present embodiment is prepared
There is silicon product excellent pore passage structure and overall structure not to destroy, and is connected with each other between nano silicon carbide granulate, nano-sized carbon
There is the hole of perforation, the nanometer silicon carbide pore-size distribution is 16-30nm, and the nanometer silicon carbide particle diameter is between silicon carbide particle
8-12nm, the specific surface area of the nanometer silicon carbide is 120-150m2/ g, the nanometer silicon carbide of the method synthesis have superelevation
Specific surface area and excellent pore structure, therefore the porous nano carborundum of the present invention industrially can be mass produced and applied.
Embodiment 3
(1) 12 grams of phenolic resin and 5.8 grams of sodium acid carbonates are weighed in beaker, add 92 milliliters of absolute ethyl alcohol, stirring
It is allowed to dissolve, under agitation, adds 50 milliliters of ethyl orthosilicates and 4.6 grams of oxalic acid, at room temperature teos hydrolysis
36h, forms SiO2Colloidal sol.
(2) in SiO2Colloidal sol adds 3.8 grams of curing agent hexamethylenetetramines, accelerates colloidal sol solidification, forms gel, Ran Hou
Dry 36h, obtains SiO under the conditions of 130 DEG C2Xerogel, then by SiO2Xerogel is accompanied in 850 DEG C of Muffle furnaces burns 12h, then removes
Template phenolic resin is removed, obtains porous SiO2。
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 2 mixing, CO gas is continuously passed through
Body, 1450 DEG C are heated to the heating rate of 6 DEG C/min, and constant temperature 12h, is cooled to room temperature, obtain initial product, then will initially produce
Thing aoxidizes 6h in 700 DEG C of air, soaks 36h after cooling and then in the hydrochloric acid and the mixed acid of hydrofluoric acid that volume ratio is 1: 3,
Then use and washed in deionized water 10 times, 12h is finally dried in 140 DEG C of drying box.
It is embodiment 3 based on nanometer silicon carbide made from the present embodiment method.
Phenetic analysis is carried out to the porous nano silicon-carbide particle being prepared：
From the XRD diffracting spectrums of embodiment 3, in 35.6 °, 60 ° and 71.8 ° of three strongest peak and carborundum
(JCPDSNo.29-1129) three strongest peak is corresponding, and substantially without dephasign.
Knowable to the adsorption and desorption curve and pore size distribution curve of embodiment 3, the carbonization that the present embodiment is prepared
There is silicon product excellent pore passage structure and overall structure not to destroy, and is connected with each other between nano silicon carbide granulate, nano-sized carbon
There is the hole of perforation, the nanometer silicon carbide pore-size distribution is 16-32nm, and the nanometer silicon carbide particle diameter is between silicon carbide particle
10-14nm, the specific surface area of the nanometer silicon carbide is 135-155m2/ g, the nanometer silicon carbide of the method synthesis have superelevation
Specific surface area and excellent pore structure, therefore the present invention porous nano carborundum industrially can mass produce and answer
With.
Embodiment 4
(1) 12 grams of phenolic resin and 4.8 grams of sodium acid carbonates are weighed in beaker, add 60 milliliters of absolute ethyl alcohol, stirring
It is allowed to dissolve, under agitation, adds 60 milliliters of ethyl orthosilicates and 4.8 grams of oxalic acid, at room temperature teos hydrolysis
36h, forms SiO2Colloidal sol.
(2) in SiO2Colloidal sol adds 3.8 grams of curing agent hexamethylenetetramines, accelerates colloidal sol solidification, forms gel, Ran Hou
Dry 36h, obtains SiO under the conditions of 120 DEG C2Xerogel, then by SiO2Xerogel is accompanied in 850 DEG C of Muffle furnaces burns 12h, then removes
Template phenolic resin is removed, obtains porous SiO2。
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 3 mixing, CO gas is continuously passed through
Body, 1450 DEG C are heated to the heating rate of 8 DEG C/min, and constant temperature 10h, is cooled to room temperature, obtain initial product, then will initially produce
Thing aoxidizes 8h in 650 DEG C of air, soaks 36h after cooling and then in the hydrochloric acid and the mixed acid of hydrofluoric acid that volume ratio is 1: 4,
Then use and washed in deionized water 12 times, 14h is finally dried in 130 DEG C of drying box.
It is embodiment 4 based on nanometer silicon carbide made from the present embodiment method.
Phenetic analysis is carried out to the porous nano silicon-carbide particle being prepared：
From the XRD diffracting spectrums of embodiment 4, in 35.6 °, 60 ° and 71.8 ° of three strongest peak and carborundum
(JCPDSNo.29-1129) three strongest peak is corresponding, and substantially without dephasign.
Knowable to the adsorption and desorption curve and pore size distribution curve of embodiment 4, the carbonization that the present embodiment is prepared
There is silicon product excellent pore passage structure and overall structure not to destroy, and is connected with each other between nano silicon carbide granulate, nano-sized carbon
There is the hole of perforation, the nanometer silicon carbide pore-size distribution is 16-35nm, and the nanometer silicon carbide particle diameter is between silicon carbide particle
8-14nm, the specific surface area of the nanometer silicon carbide is 110-1160m2/ g, the nanometer silicon carbide of the method synthesis have superelevation
Specific surface area and excellent pore structure, therefore the present invention porous nano carborundum industrially can mass produce and answer
With.
Embodiment 5
(1) 12 grams of phenolic resin and 6 grams of sodium acid carbonates are weighed in beaker, add 8.3 milliliters of absolute ethyl alcohol, stirring makes
Dissolving, under agitation, add 40 milliliters of ethyl orthosilicates and 3.6 grams of oxalic acid, at room temperature teos hydrolysis 36h,
Form SiO2Colloidal sol.
(2) in SiO2Colloidal sol adds 2.8 grams of curing agent hexamethylenetetramines, accelerates colloidal sol solidification, forms gel, Ran Hou
Dry 48h, obtains SiO under the conditions of 130 DEG C2Xerogel, then by SiO2Xerogel is accompanied in 850 DEG C of Muffle furnaces burns 10h, then removes
Template phenolic resin is removed, obtains porous SiO2。
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 4 mixing, CO gas is continuously passed through
Body, 1450 DEG C are heated to the heating rate of 10/min, and constant temperature 10h, is cooled to room temperature, obtain initial product, then will initially produce
Thing aoxidizes 12h in 700 DEG C of air, is soaked after cooling and then in the hydrochloric acid and the mixed acid of hydrofluoric acid that volume ratio is 1: 4
36h, then with being washed in deionized water 11 times, finally dries 12h in 180 DEG C of drying box.
It is embodiment 5 based on nanometer silicon carbide made from the present embodiment method.
Phenetic analysis is carried out to the porous nano silicon-carbide particle being prepared：
From the XRD diffracting spectrums of embodiment 5, in 35.6 °, 60 ° and 71.8 ° of three strongest peak and carborundum
(JCPDSNo.29-1129) three strongest peak is corresponding, and substantially without dephasign.
Knowable to the adsorption and desorption curve and pore size distribution curve of embodiment 5, the carbonization that the present embodiment is prepared
There is silicon product excellent pore passage structure and overall structure not to destroy, and is connected with each other between nano silicon carbide granulate, nano-sized carbon
There is the hole of perforation, the nanometer silicon carbide pore-size distribution is 16-30nm, and the nanometer silicon carbide particle diameter is between silicon carbide particle
8-12nm, the specific surface area of the nanometer silicon carbide is 120-150m2/ g, the nanometer silicon carbide of the method synthesis have superelevation
Specific surface area and excellent pore structure, therefore the porous nano carborundum of the present invention industrially can be mass produced and applied.
Embodiment 6
(1) 12 grams of phenolic resin and 9.6 grams of sodium acid carbonates are weighed in beaker, add 96 milliliters of absolute ethyl alcohol, stirring
It is allowed to dissolve, under agitation, adds 96 milliliters of ethyl orthosilicates and 3.6 grams of oxalic acid, at room temperature teos hydrolysis
72h, forms SiO2Colloidal sol.
(2) in SiO2Colloidal sol adds 6 grams of curing agent hexamethylenetetramines, accelerates colloidal sol solidification, forms gel, Ran Hou
Dry 48h, obtains SiO under the conditions of 180 DEG C2Xerogel, then by SiO2Xerogel is accompanied in 1000 DEG C of Muffle furnaces burns 12h, then removes
Template phenolic resin is removed, obtains porous SiO2。
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 5 mixing, CO gas is continuously passed through
Body, 1500 DEG C are heated to the heating rate of 12 DEG C/min, and constant temperature 10h, is cooled to room temperature, obtain initial product, then will be initial
Product aoxidizes 6h in 650 DEG C of air, is soaked after cooling and then in the hydrochloric acid and the mixed acid of hydrofluoric acid that volume ratio is 1: 3
36h, then with being washed in deionized water 12 times, finally dries 12h in 220 DEG C of drying box.
It is embodiment 6 based on nanometer silicon carbide made from the present embodiment method.
Phenetic analysis is carried out to the porous nano silicon-carbide particle being prepared：
From the XRD diffracting spectrums of embodiment 6, in 35.6 °, 60 ° and 71.8 ° of three strongest peak and carborundum
(JCPDSNo.29-1129) three strongest peak is corresponding, and substantially without dephasign.
Knowable to the adsorption and desorption curve and pore size distribution curve of embodiment 6, the carbonization that the present embodiment is prepared
There is silicon product excellent pore passage structure and overall structure not to destroy, and is connected with each other between nano silicon carbide granulate, nano-sized carbon
There is the hole of perforation, the nanometer silicon carbide pore-size distribution is 16-30nm, and the nanometer silicon carbide particle diameter is between silicon carbide particle
8-12nm, the specific surface area of the nanometer silicon carbide is 120-150m2/ g, the nanometer silicon carbide of the method synthesis have superelevation
Specific surface area and excellent pore structure, therefore the porous nano carborundum of the present invention industrially can be mass produced and applied.
Above example technical solution using the present invention have it is simple to equipment requirement, process is easily operated, product is all
The advantages of phase is short, and the method for preparing nanometer silicon carbide cost-effective can obtain the required nano silicon carbide in this area
Silicon.
Finally it should be noted that the above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, to the greatest extent
Pipe is described in detail the present invention with reference to above-described embodiment, and those of ordinary skill in the art still can be to this hair
Bright embodiment technical scheme is modified or replaced equivalently, these without departing from the spirit and scope of the present invention any modification or
Person's equivalent substitution, is applying within pending claims.
Claims (10)
1. a kind of nanometer silicon carbide, it is characterised in that the nanometer silicon carbide pore-size distribution is 16-48nm, the nano silicon carbide
Silicon grain footpath is 8-16nm, and the specific surface area of the nanometer silicon carbide is 120-180m2/ g, between the particle of the nanometer silicon carbide
Pore structure with multidimensional hydridization.
2. a kind of preparation method of nanometer silicon carbide, the nanometer silicon carbide is the nanometer silicon carbide described in claim 1, it is special
Sign is that the preparation method includes the following steps：
(1) solvent that 5-8 parts by weight are added in the surfactant of 1 parts by weight and the carbonate of 0.3-0.8 parts by weight is taken, then
Under conditions of stirring, the ethyl orthosilicate of 3-8 parts by weight and the catalyst of 0.1-0.3 parts by weight are added, at room temperature positive silicic acid
Ethyl ester hydrolyzes 12-72h, forms SiO2Colloidal sol；
(2) in SiO2Colloidal sol adds the set agent of 0.2-0.5 parts by weight, forms SiO2Gel, it is then dry at 80 DEG C -180 DEG C
24-48h forms SiO2Xerogel, then by SiO2Xerogel is obtained porous in 750 DEG C of -1000 DEG C of Muffle kiln roasting 4-12h
SiO2；
(3) by porous SiO2It is porous SiO in molar ratio with graphite powder2: graphite powder=1：After 1-5 mixing, CO gas is continuously passed through
Body, is heated to 1350 DEG C -1500 DEG C, constant temperature 8-36h, is cooled to room temperature, is initially produced with the heating rate of 5-12 DEG C/min
Thing, then by initial product through peroxidating, acid soak, wash and be dried to obtain nanometer silicon carbide.
3. the preparation method of nanometer silicon carbide as claimed in claim 2, it is characterised in that the surfactant is phenolic aldehyde tree
In fat, hexadecyltrimethylammonium chloride, cetyl trimethylammonium bromide, polyethylene glycol, biphenyl, furfural, saccharide compound
At least one.
4. the preparation method of nanometer silicon carbide as claimed in claim 3, it is characterised in that the saccharide compound is sucrose, fruit
At least one of sugar, fructose.
5. the preparation method of nanometer silicon carbide as claimed in claim 2, it is characterised in that the catalyst is oxalic acid, hydrochloric acid, nitre
Acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide or ammonium hydroxide.
6. the preparation method of nanometer silicon carbide as claimed in claim 2, it is characterised in that the carbonate is sodium carbonate, carbon
At least one of sour potassium, sodium acid carbonate, saleratus.
7. the preparation method of nanometer silicon carbide as claimed in claim 2, it is characterised in that the granularity of the graphite powder is 45-200
μm, the carbon content of the graphite powder is ＞ 99.5%.
8. the preparation method of nanometer silicon carbide as claimed in claim 2, it is characterised in that the set agent is six methines four
At least one of amine, resol, amino resins.
9. the preparation method of nanometer silicon carbide as claimed in claim 2, it is characterised in that the condition of the oxidation is：Temperature is
600-900 DEG C, time 4-12h；The condition of the acid soak is：Time is 24-120h；The condition of the washing is：Go
Ion water washing 8-16 times；The condition of the drying is：Temperature is 110-220 DEG C, time 12-24h.
10. the preparation method of nanometer silicon carbide as claimed in claim 2, it is characterised in that the acid solution is that volume ratio is 1：
The hydrochloric acid of 2-5 and the mixed acid of hydrofluoric acid.
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