CN109824362A - Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing - Google Patents
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing Download PDFInfo
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Abstract
The present invention relates to biomass carbon SiClx/carbon composites and preparation method thereof of step firing.Its technical solution is: the catalyst of the silicon source of 95~99wt% and 1~5wt% are mixed to get mixture；It is 3~5mol/L according to concentration, the mixture is placed in ethanol solution, mixed solution is made；Biomass porous carbon template is placed in the mixed solution again, at the uniform velocity stirs 1~3h with magnetic stirring apparatus under the conditions of -0.05~-0.04MPa, is then placed in vacuum drying oven, 1150~1350 DEG C are heated under the conditions of -0.15~-0.1MPa, keeps the temperature 3~7h；Natural cooling obtains biomass carbon SiClx/carbon composite of step firing.The present invention has the characteristics that simple process, reaction temperature are low, at low cost and easy to industrialized production, and the biomass carbon SiClx being burnt into a step prepared by this method/carbon composite porosity is high, pattern is good and corrosion-resistant.
Description
Technical field
The invention belongs to biomass carbon SiClx/carbon composite technical fields.More particularly to the biomass of step firing
Silicon carbide/carbon composite material and preparation method thereof.
Background technique
Carborundum porous ceramics have the advantages that high rigidity, high intensity, corrosion-resistant and large specific surface area, are widely used in
Catalyst carrier, heating device, filter device and insulation etc..Existing porous ceramic film material preparation method has colloidal sol
Gel method, Polymeric sponge method and granulation mass area method etc., though these methods have, process is simple, the period is short and can give birth on a large scale
The features such as production, but the porous ceramics stomata arrangement prepared is mixed and disorderly, size is uneven and voidage is lower.In order to prepare different-shape
Porous ceramics, need to artificially add pore creating material or carry out following process molding, this considerably increases production costs, and due to having
The presence of machine object will also result in pollution to environment.
Currently, since natural wood internal structure is unique, resourceful and cheap, using plant as templated synthesis
Porous material receives more and more attention.Possess by the wood of cellulose, hemicellulose and the formed Cell microstructure of lignin
Material, which is heated, is made carbon templated porous frame.Prepared by porous ceramics and existing method using the preparation of carbon templated porous frame
Porous material is compared, and not only porosity is high, large specific surface area and corrosion-resistant etc., and plant carbon template has natural orderly gas
Hole, therefore plant carbon template can better meet the demand of different shape size, have better application prospect.
O.Gryshkov etc. (O.Gryshkov, N.I.Klyui, V.P.Temchenko, V.S.Kyselov,
A.Chatterjee,A.E.Belyaev,L.Lauterboeck,D.Larmolenko,B.Glasmacher.Porous
biomorphic silicon carbide ceramics coated with hydroxyapatite as prospective
materials for bone implants.Materials Science and Engineering C,2016,68:143-
152) log is made in 900 DEG C of progress carbonization treatments under inert gas atmosphere as carbon source by carbon mould using linden or pear wood
Plate；Then siliconising is carried out under vacuum conditions, and is warming up to 1900 DEG C with 10~20 DEG C/min rate, keeps the temperature 2h, though it is made
Carborundum porous ceramics.But the disadvantages of high, energy consumption that there are reaction temperatures is greatly and purity is not high.
(J.Ding, H.X.Zhu, G.Q.Li, C.J.Deng, J.Li.Growth of the SiC nanowires such as J.Ding
on wooden template surface using molten salt media.Applied Surface Science,
2014,320:620-626) molten-salt growth method is used, using platane wood as carbon template, KCl and KF are as fused salt；By platane wood in argon gas
It is heated to 900 DEG C under atmosphere, keeps the temperature 3h, obtains carbon template.Carbon template is placed in the mixed powder of complex salt and silicon powder support again,
It is warming up to 1200~1400 DEG C under an argon atmosphere, silicon carbide nanometer line is made." one kind generates one in multiporous biological carbon template
The method for tieing up silicon carbide nanometer line " (CN103318891A) patented technology, proposes Nacl and silicon source in planetary ball mill
Mixed powder is made in 10~60min of middle mixing；Then mixed powder and porous carbon template are heated to 1250 under an argon atmosphere
~1400 DEG C, 2~10h is kept the temperature, one-dimensional silicon carbide nanometer line is made.Both methods and sol-gal process, chemical vapor infiltration
Method is compared with conventional methods such as foamings, though synthesis temperature is lower, silicon powder can not be coated uniformly in carbon template, causes to react
Not exclusively, and at high temperature fused salt is volatile, and reaction process is uncontrollable.
A kind of " preparation method of biomass-based porous silicon carbide absorbing material " (CN104961493A) patented technology, the skill
Fruit pulp after silicon powder and carbonization is placed in tube furnace by art using fruit pulp as carbon source, logical with 10~60mL/min rate
Enter argon gas；Under an argon atmosphere, 1000 DEG C are first first warming up to 5 DEG C/min rate, are then heated to 10 DEG C/min rate
1300~1800 DEG C, 1~8h is kept the temperature, silicon carbide is made.This method reaction temperature is higher, soaking time is longer and energy consumption is high.
A kind of " preparation method of the spherical porous thyrite of biological structure " (CN1830901A) patented technology, should
Silicon powder is first placed in vacuum drying oven bottom using crops fruit as carbon source by technology, and carbon source is placed in vacuum drying oven upper layer, it is heated to 1500~
2000 DEG C of progress gas phase siliconisings；It is heated to 600~800 DEG C of progress carbon elimination processing in air, is then washed, is obtained with acid
To porous silicon carbide ceramic.But there are silicon powders to come into full contact with carbon source for this method, and silicon carbide in carbon template is caused to be distributed not
Equal disadvantage；And liquid-phase silicone or gas-phase silicon can be attached on the silicon carbide grown, cause product impure, using acid to sample
Carrying out cleaning can cause environmental pollution.And required reaction temperature height and energy consumption is high.
There is the disadvantages of synthesis temperature is high, experiment flow is cumbersome and soaking time is long in above method, increase its life mostly
Produce cost.
Summary of the invention
The present invention is directed to overcome existing technological deficiency, it is therefore an objective to it is low and be easy to industry to provide a kind of simple process, production cost
Biomass carbon SiClx/carbon composite the preparation method for the step firing that metaplasia produces.It is burnt into the step that this method obtains
The advantages that biomass carbon SiClx/carbon composite porosity is high, pattern is good and corrosion-resistant.
To achieve the above object, the technical solution adopted by the present invention is that: by the silicon source of 95~99wt% and 1~5wt%
Catalyst mixes to get mixture；It is 3~5mol/L according to concentration, the mixture is placed in ethanol solution, mixing is made
Solution；Biomass porous carbon template is placed in the mixed solution again, magnetic agitation under the conditions of -0.05~-0.04MPa
Device at the uniform velocity stirs 1~3h, is then placed in vacuum drying oven, and 1150~1350 DEG C are heated under the conditions of -0.15~-0.1MPa, protects
3~7h of temperature；Natural cooling obtains biomass carbon SiClx/carbon composite of step firing.
The partial size of the silicon source is less than 10 μm；The silicon source is silicon powder or is silicon dioxide powder, Si content in the silicon powder
Greater than 99.0wt%, SiO in the silicon dioxide powder2Content is greater than 99.0wt%.
The catalyst is one of ferric nitrate, cobalt nitrate and nickel nitrate；The purity of the catalyst is greater than
98.5wt%.
The purity of the ethyl alcohol is greater than 99.7wt%.
The biomass porous carbon template the preparation method comprises the following steps: by pine be placed in tube furnace in, in -0.15~-0.1MPa
Under the conditions of, 600~650 DEG C are warming up to the rate of 1~1.5 DEG C/min, keeps the temperature 1~2h；Again with the rate liter of 2~3 DEG C/min
Temperature keeps the temperature 1~3h, is then down to room temperature with the rate of 2~3 DEG C/min, obtains biomass porous carbon mould to 800~1000 DEG C
Plate.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art:
First mixed solution will be made in silicon source and catalyst merging ethanol solution in the present invention, then by biomass porous carbon mould
Plate is placed in mixed solution, is at the uniform velocity stirred under the conditions of -0.05~-0.04Mpa using magnetic stirring apparatus；After impregnating again
Biomass porous carbon template keeps the temperature 3~7h under the conditions of 1150~1350 DEG C, and the biomass carbon of step firing is made in natural cooling
SiClx/carbon composite.This method simple process, reaction temperature are low, raw material easily obtains, at low cost and easy to industrialized production.
The present invention is due to penetrating into biomass porous carbon for raw material and catalyst using magnetic stirring apparatus under condition of negative pressure
In template, compared with the existing technology, particle can more evenly and effectively penetrate into carbon template opening stomata；The addition energy of catalyst
Reaction temperature is effectively reduced and shortens soaking time；Biomass carbon SiClx/carbon composite, technique are prepared using a step sintering method
Simply, easy to industrialized production, the biomass carbon SiClx/carbon composite large specific surface area and intensity of the step firing of preparation
Height, therefore can preferably be applied to catalyst carrier etc..
The silicon carbide that the present invention is grown in biomass porous carbon template physically well develops, structural integrity.And the carbon mould used
Plate only changes its chemical component, does not change its basic structure, and porosity is high, pattern is good and corrosion-resistant.
Therefore, the present invention has the characteristics that simple process, reaction temperature are low, at low cost and easy to industrialized production, with this
Biomass carbon SiClx/carbon composite porosity of the step firing of method preparation is high, pattern is good and corrosion-resistant.
Detailed description of the invention
Fig. 1 is biomass carbon SiClx/carbon composite XRD diagram piece of a step prepared by the present invention firing；
Fig. 2 is biomass carbon SiClx/carbon composite SEM picture of a step shown in FIG. 1 firing.
Specific embodiment
Below with reference to specific implementation method, the invention will be further described, not to the limitation of its protection scope.
To avoid repeating, first by the preparation method of material involved in present embodiment and biomass porous carbon template
Unify legislation is as follows, repeats no more in embodiment:
The partial size of the silicon source is less than 10 μm；Si content is greater than 99.0wt% in the silicon powder, in the silicon dioxide powder
SiO2Content is greater than 99.0wt%.
The purity of the catalyst is greater than 98.5wt%.
The purity of the ethyl alcohol is greater than 99.7wt%.
The biomass porous carbon template the preparation method comprises the following steps: by pine be placed in tube furnace in, in -0.15~-0.1MPa
Under the conditions of, 600~650 DEG C are warming up to the rate of 1~1.5 DEG C/min, keeps the temperature 1~2h；Again with the rate liter of 2~3 DEG C/min
Temperature keeps the temperature 1~3h, is then down to room temperature with the rate of 2~3 DEG C/min, obtains biomass porous carbon mould to 800~1000 DEG C
Plate.
Embodiment 1
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing.Preparation method described in the present embodiment is:
The catalyst of the silicon source of 95~97wt% and 3~5wt% are mixed to get mixture；According to concentration be 3~
The mixture is placed in ethanol solution by 4mol/L, and mixed solution is made；Biomass porous carbon template is placed in again described mixed
It closes in solution, at the uniform velocity stirs 1~2h with magnetic stirring apparatus under the conditions of -0.05~-0.04MPa, be then placed in vacuum drying oven,
It is heated to 1150~1250 DEG C under the conditions of -0.15~-0.1MPa, keeps the temperature 3~5h；Natural cooling obtains the life of step firing
Substance silicon carbide/carbon composite material.
The catalyst is ferric nitrate；
The silicon source is silicon powder.
Embodiment 2
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing.The present embodiment in addition to following materials,
Remaining same embodiment 1:
The catalyst is cobalt nitrate；
The silicon source is silicon dioxide powder.
Example example 3
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing.The present embodiment in addition to following materials,
Remaining same embodiment 1:
The catalyst is nickel nitrate；
The silicon source is silicon powder.
Embodiment 4
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing, the present embodiment in addition to following materials,
Remaining same embodiment 1:
The catalyst is ferric nitrate；
The silicon source is silicon dioxide powder.
Embodiment 5
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing.Preparation method described in the present embodiment is:
The catalyst of the silicon source of 97~99wt% and 1~3wt% are mixed to get mixture；According to concentration be 4~
The mixture is placed in ethanol solution by 5mol/L, and mixed solution is made；Biomass porous carbon template is placed in again described mixed
It closes in solution, at the uniform velocity stirs 2~3h with magnetic stirring apparatus under the conditions of -0.05~-0.04MPa, be then placed in vacuum drying oven,
It is heated to 1250~1350 DEG C under the conditions of -0.15~-0.1MPa, keeps the temperature 5~7h；Natural cooling obtains the life of step firing
Substance silicon carbide/carbon composite material.
The catalyst is cobalt nitrate；
The silicon source is silicon powder.
Embodiment 6
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing, the present embodiment in addition to following materials,
Remaining same embodiment 5:
The catalyst is nickel nitrate；
The silicon source is silicon dioxide powder.
Embodiment 7
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing, the present embodiment in addition to following materials,
Remaining same embodiment 5:
The catalyst is ferric nitrate；
The silicon source is silicon powder.
Embodiment 8
Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing, the present embodiment in addition to following materials,
Remaining same embodiment 5:
The catalyst is nickel nitrate；
The silicon source is silicon dioxide powder.
Present embodiment has following good effect compared with prior art:
First mixed solution will be made in silicon source and catalyst merging ethanol solution in present embodiment, then by biomass
Porous carbon template is placed in mixed solution, is at the uniform velocity stirred under the conditions of -0.05~-0.04Mpa using magnetic stirring apparatus；Again
Biomass porous carbon template keeps the temperature 3~7h under the conditions of 1150~1350 DEG C after impregnating, natural cooling, and step firing is made
Biomass carbon SiClx/carbon composite.This method simple process, reaction temperature are low, raw material easily obtains, it is at low cost and be easy to industry
Metaplasia produces.
Present embodiment is due to penetrating into biology for raw material and catalyst using magnetic stirring apparatus under condition of negative pressure
In matter porous carbon template, compared with the existing technology, particle can more evenly and effectively penetrate into carbon template opening stomata；Catalyst
Addition can be effectively reduced reaction temperature and shorten soaking time；It is compound that biomass carbon SiClx/carbon is prepared using a step sintering method
Material, simple process, easy to industrialized production, biomass carbon SiClx/carbon composite specific surface area of the step firing of preparation
Big and intensity is high, therefore can preferably be applied to catalyst carrier etc..
The silicon carbide that present embodiment is grown in biomass porous carbon template physically well develops, structural integrity.And it adopts
Carbon template only changes its chemical component, does not change its basic structure, and porosity is high, pattern is good and corrosion-resistant.
Biomass carbon SiClx/carbon composite of the step firing of present embodiment preparation is as depicted in figs. 1 and 2,
Fig. 1 is biomass carbon SiClx/carbon composite XRD diagram of one step of one kind firing prepared by embodiment 1, and Fig. 2 is shown in FIG. 1 one
Biomass carbon SiClx/carbon composite SEM figure of step firing.As shown in Figure 1, the biomass carbonization of prepared step firing
Silicon/carbon composite is pure phase；As shown in Figure 2, biomass carbon SiClx/carbon composite pattern of prepared step firing
It is good, and the structural integrity of biomass porous carbon template.
Therefore, present embodiment has simple process, the spy that reaction temperature is low, at low cost and easy to industrialized production
Point, the biomass carbon SiClx being burnt into a step prepared by this method/carbon composite porosity is high, pattern is good and corrosion-resistant.
Claims (6)
1. biomass carbon SiClx/carbon composite preparation method of step firing, is characterized in that the silicon source of 95~99wt%
It mixes with the catalyst of 1~5wt% to get mixture；It is 3~5mol/L according to concentration, it is molten that the mixture is placed in ethyl alcohol
In liquid, mixed solution is made；Biomass porous carbon template is placed in the mixed solution again, in -0.05~-0.04MPa item
1~3h is at the uniform velocity stirred with magnetic stirring apparatus under part, is then placed in vacuum drying oven, is heated under the conditions of -0.15~-0.1MPa
1150~1350 DEG C, keep the temperature 3~7h；Natural cooling obtains biomass carbon SiClx/carbon composite of step firing.
2. biomass carbon SiClx/carbon composite preparation method of step firing according to claim 1, feature exist
In the silicon source partial size less than 10 μm；The silicon source is silicon powder or is silicon dioxide powder, and Si content is greater than in the silicon powder
99.0wt%, SiO in the silicon dioxide powder2Content is greater than 99.0wt%.
3. biomass carbon SiClx/carbon composite preparation method of step firing according to claim 1, feature exist
In the catalyst be one of ferric nitrate, cobalt nitrate and nickel nitrate；The purity of the catalyst is greater than 98.5wt%.
4. biomass carbon SiClx/carbon composite preparation method of step firing according to claim 1, feature exist
It is greater than 99.7wt% in the purity of the ethyl alcohol.
5. biomass carbon SiClx/carbon composite preparation method of step firing according to claim 1, feature exist
In the biomass porous carbon template the preparation method comprises the following steps: by pine be placed in tube furnace in, under the conditions of -0.15~-0.1MPa,
600~650 DEG C are warming up to the rate of 1~1.5 DEG C/min, keeps the temperature 1~2h；800 are warming up to again with the rate of 2~3 DEG C/min
~1000 DEG C, 1~3h is kept the temperature, room temperature is then down to the rate of 2~3 DEG C/min, obtains biomass porous carbon template.
6. a kind of biomass carbon SiClx/carbon composite of step firing, it is characterised in that the biomass of the step firing
Silicon carbide/carbon composite material is that biomass carbon SiClx/carbon of the firing of a step according to any one of right 1~5 is multiple
Biomass carbon SiClx/carbon composite of the firing of a step prepared by the preparation method of condensation material.
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| CN111410196A (en) * | 2020-03-31 | 2020-07-14 | 青海大学 | Porous SiC material, preparation method thereof and phase change energy storage material |
| CN113800945A (en) * | 2021-09-27 | 2021-12-17 | 南京航空航天大学 | Loofah derived porous silicon carbide ceramic-based high-temperature photo-thermal storage material and preparation method thereof |
| CN115246646A (en) * | 2021-12-22 | 2022-10-28 | 浙江理工大学 | Method for preparing silicon carbide nano-wire by using renewable resources or wastes as carbon source |
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Application publication date: 20190531 |