CN104876621A - C/SiC porous composite ceramic with bionic structure and preparation method of C/SiC porous composite ceramic - Google Patents
C/SiC porous composite ceramic with bionic structure and preparation method of C/SiC porous composite ceramic Download PDFInfo
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Abstract
The invention provides a C/SiC porous composite ceramic with a bionic structure and a preparation method of the C/SiC porous composite ceramic. The C/SiC porous composite ceramic is prepared by the following steps: by taking carbon fibers as a skeleton, depositing carbon microspheres on the surfaces of the carbon fibers by adopting a microwave hydrothermal method to construct a carbon fiber network skeleton; reacting the microspheres on the surfaces of the carbon fibers with gas phase SiO by using carbon thermal reduction reaction to generate SiC, inherit microstructures of the carbon microspheres, and form SiC microspikes on the surfaces of the carbon fibers; and meanwhile, forming SiC nano fuzzes (SiC nano wires) on the surface of the SiC microspikes by using the reaction between gas phase SiO and CO, thereby constructing the C/SiC porous composite ceramic with the bionic structure. The construction of the bionic structure can greatly improve the specific area of the SiC porous ceramic and ensure that the SiC porous ceramic has potential applications in the fields of catalyst carrier materials and high-temperature gas filtration.
Description
Technical field
The invention belongs to porous ceramic film material preparing technical field, relate to one and there is biomimetic features C/SiC porous composite ceramics and preparation method thereof.
Background technology
The chemical stability that silicon carbide (SiC) has not only had, high physical strength and hardness, and there is good heat-conductivity conducting performance.Especially the electrical and thermal conductivity that SiC is good is conducive to the heat trnasfer of catalyzer in reaction process and the electron transmission between catalyst activity component and carrier, becomes the ideal material of support of the catalyst.But, in chemical industry catalysis technical field, but seldom see the figure that SiC porous ceramics is applied.Tracing it to its cause, is because its specific surface area of SiC porous ceramics that commercial methods is produced is difficult to meet the requirement of catalyst support material.Therefore, how to prepare the high-specific surface area SiC that can be used as support of the catalyst, caused the attention of investigator, relevant research is also increasing, develops the methods such as template, sol-gel method, Polycarbosilane cracking process, has prepared SiC porous particle, SiC nanotube, the structures such as SiC microballoon.Chinese invention patent 02130064.X reports a kind of high-specific surface area silicon carbide and preparation method thereof, and the diameter of the high-specific surface area silicon carbide prepared by the method is 10-20nm, and specific surface area is 60-160m
2/ g, pore size distribution range is 3-100nm.But high-specific surface area SiC prepared by aforesaid method will reach practical application also to be needed shaping, the support of the catalyst made is made to have suitable shape, size and physical strength, to meet the operational requirement of industrial reactor.In the process of shaping of catalyst, the sintering process of porous SiC ceramics can cause the significantly reduction of specific surface area.Therefore, develop a kind of carborundum porous ceramics and preparation method thereof, while making it have specific area, also having stronger formability and physical strength is solve the key that this material applies in catalytic field.
Summary of the invention
Technical problem to be solved by this invention is to provide one and has biomimetic features C/SiC porous composite ceramics and preparation method thereof, C/SiC porous composite ceramics obtained by this method, while having specific area, also has stronger formability and physical strength.
A kind of preparation method with biomimetic features C/SiC porous composite ceramics, having biomimetic features C/SiC porous composite ceramics take carbon fiber as skeleton, adopt microwave-hydrothermal method at carbon fiber surface deposit carbon microballoon, to build carbon fiber network skeleton, then, carbothermic reduction reaction is utilized to form SiC at carbon fiber surface micro-prominent, then, form SiC nanometer fine hair on the micro-prominent surface of SiC, thus construct there is biomimetic features C/SiC porous composite ceramics.
The formation method of the carbosphere of described carbon fiber surface is: take carbon fiber as skeleton, take glucose as carbon source, skeleton and carbon source are positioned in micro-wave diminishing pot, react micro-wave diminishing pot being put into microwave attenuation materials instrument, temperature of reaction is 170 ~ 210 DEG C, and the reaction times is 1 ~ 3h.
The concentration of described glucose solution is 10 ~ 100g/L.
Micro-the dashing forward of described SiC utilizes carbothermic reduction reaction that carbon fiber surface carbosphere and gas phase SiO are reacted to generate SiC, and hereditary carbosphere microtexture, form SiC at carbon fiber surface micro-prominent.
Described SiC nanometer fine hair utilizes gas phase SiO and CO to react to be formed on the micro-prominent surface of SiC.
A kind of preparation method with biomimetic features C/SiC porous composite ceramics, comprise the following steps: step 1: take carbon fiber as skeleton, take glucose as carbon source, adopt microwave hydrothermal technology, glucose solution and carbon fiber skeleton are put into micro-wave diminishing pot, and then micro-wave diminishing pot is put into microwave attenuation materials instrument react, obtain the carbon fiber skeleton of carbosphere bonding; Step 2: carbon fiber skeleton step 1 obtained puts into vacuum sintering furnace, with Si and SiO
2mixed powder is as silicon source, and controlling temperature of reaction is 1300 ~ 1600 DEG C, and reaction pressure is 1 ~ 100KPa, and the reaction times is 1 ~ 4h.
In described step 2, carbon fiber skeleton is placed in Si and SiO
2above mixed powder.
The inwall close contact of described carbon fiber skeleton and sintering oven, makes reactant gases be conducive to spreading to carbon fiber skeletal internal.
One has biomimetic features C/SiC porous composite ceramics, obtains according to method preparation described above.
One has biomimetic features C/SiC porous composite ceramics, comprise carbon fiber, the carbosphere utilizing microwave hydrothermal to react formation between carbon fiber connects, carbon fiber and carbosphere are built into carbon fiber network skeleton, it is micro-prominent that described carbosphere utilizes carbothermic reduction reaction to form SiC at carbon fiber surface, is formed with SiC nanometer fine hair micro-the dashing forward of this SiC.
Compared with prior art, the present invention at least has the following advantages: present method is for thinking with nature micro-/ nano multilevel hierarchy, a kind of novel C/SiC porous composite ceramics is built from the angle of biomimetic material design, using carbon fiber as skeleton, micro-prominent with in SiC microballoon simulation organism, with nanometer fine hair in SiC nanowire simulation organism, build the C/SiC porous composite ceramics that has biomimetic features.C/SiC porous composite ceramics involved by the method has high-specific surface area, is easy to shaping, the characteristic of high strength.C/SiC porous composite ceramics is using carbon fiber as skeleton, microwave-hydrothermal method is adopted to build carbon fiber network skeleton at carbon fiber surface deposit carbon microballoon, utilize carbothermic reduction reaction that carbon fiber surface carbosphere and gas phase SiO are reacted and generate SiC, and hereditary carbosphere microtexture, form SiC micro-prominent (SiC microballoon) at carbon fiber surface; Utilize gas phase SiO and CO to react simultaneously and form SiC nanometer fine hair (SiC nanowire) on the micro-prominent surface of SiC, thus construct there is biomimetic features C/SiC porous composite ceramics.The carbosphere utilizing microwave hydrothermal to react formation between carbon fiber connects, and forming the three-dimensional net structure of a high porosity, high strength, in conjunction with the feature of carbon fiber high-strength light, is the basis of C/SiC porous composite ceramics; Simulate the micro-prominent and nanometer fine hair of organism with SiC microballoon and SiC nanowire, achieve the Bionic Design of C/SiC porous composite ceramics.The structure of this biomimetic features, significantly can improve the specific surface area of SiC porous ceramics, makes it have potential application at catalyst support material and high temperature air filtration field.
Accompanying drawing explanation
Fig. 1 is C/SiC porous composite ceramic structures schematic diagram of the present invention; A () is the three-dimensional structure unit of C/SiC porous composite ceramics; B () is individual carbon fibers surface microstructure schematic diagram in (a); C () (d) (e) is respectively the schematic diagram of carbon fiber, SiC microballoon and SiC nanowire in (b).
Fig. 2 is the SEM shape appearance figure of C/SiC porous composite ceramics preparation process different steps: the reaction of (a) Microwave Water is at the carbosphere of carbon fiber surface synthesis, the SiC layer of (b) carbon fiber surface and SiC microballoon (micro-prominent), the micro-prominent enlarged view of single SiC in (c) figure (b), the SiC nanowire (fine hair) on the micro-prominent surface of SiC when () reaction times is 1h d, the SiC nanowire (fine hair) on SiC micro-prominent surface when (e) reaction times is 3h.
Embodiment
The inventive method is for thinking with nature micro-/ nano multilevel hierarchy, a kind of novel C/SiC porous composite ceramics is built from the angle of biomimetic material design, using carbon fiber as skeleton, micro-prominent with in SiC microballoon simulation organism, with nanometer fine hair in SiC nanowire simulation organism, build the C/SiC porous composite ceramics that has biomimetic features.C/SiC porous composite ceramics involved by the method has high-specific surface area, is easy to shaping, the characteristic of high strength.C/SiC porous composite ceramics is using carbon fiber as skeleton, microwave-hydrothermal method is adopted to build carbon fiber network skeleton at carbon fiber surface deposit carbon microballoon, utilize carbothermic reduction reaction that carbon fiber surface carbosphere and gas phase SiO are reacted and generate SiC, and hereditary carbosphere microtexture, form SiC micro-prominent (SiC microballoon) at carbon fiber surface; Utilize gas phase SiO and CO to react simultaneously and form SiC nanometer fine hair (SiC nanowire) on the micro-prominent surface of SiC, thus construct there is biomimetic features C/SiC porous composite ceramics.The carbosphere utilizing microwave hydrothermal to react formation between carbon fiber connects, and forming the three-dimensional net structure of a high porosity, high strength, in conjunction with the feature of carbon fiber high-strength light, is the basis of C/SiC porous composite ceramics; Simulate the micro-prominent and nanometer fine hair of organism with SiC microballoon and SiC nanowire, achieve the Bionic Design of C/SiC porous composite ceramics.
The invention provides one and there is biomimetic features C/SiC porous composite ceramics and preparation method thereof, comprise the steps:
Step 1: choose carbon fiber skeleton, carbon fiber skeleton can be chopped carbon fiber prefabricated component, carbon fiber stereo fabric, and density can at 0.2 ~ 0.6g/cm
3;
Step 2: prepare carbosphere in the carbon fiber skeleton that step 1 is chosen.Adopt microwave hydrothermal technology, biomass carbon source solution and carbon fiber skeleton are put into micro-wave diminishing pot, and then micro-wave diminishing pot is put into microwave attenuation materials instrument and react, obtain the carbon fiber skeleton that carbosphere bonds.The parameter of microwave hydrothermal reaction is: biomass carbon source strength of solution controls at 10 ~ 100g/L, and temperature of reaction is 170 ~ 210 DEG C, and the reaction times is 1 ~ 3h, and carbosphere size control is at 200 ~ 500nm;
Step 3: the porous carbon template after step 2 being processed, puts into vacuum sintering furnace.With Si and SiO
2mixed powder as silicon source, Si:SiO
2mol ratio controls between 2:1 ~ 2:3, and temperature of reaction controls between 1300 ~ 1600 DEG C, and reaction point pressure-controlled is between 1 ~ 100KPa, and the reaction times controls at 1 ~ 4h.During reaction, porous carbon template is placed in Si and SiO
2above mixed powder, and porous carbon template and reaction vessel inwall close contact, reactant gases is conducive to porous carbon template internal diffusion.
Embodiment 1:
Step 1: choosing density is 0.2g/cm
3chopped carbon fiber prefabricated component as skeleton; Using glucose as carbon source, compound concentration is the glucose solution of 50g/L;
Step 2: adopt microwave hydrothermal technology, glucose solution and carbon fiber skeleton are put into micro-wave diminishing pot, and then micro-wave diminishing pot is put into microwave attenuation materials instrument and react, obtain the carbon fiber skeleton that carbosphere bonds.Temperature of reaction controls at 170 DEG C, and the reaction times controls at 1h, and final carbosphere is of a size of 200nm.
Step 3: the porous carbon template after step 2 being processed, puts into vacuum sintering furnace.With Si and SiO
2mixed powder as silicon source, Si:SiO
2mol ratio controls at 2:1, and temperature of reaction controls at 1300 DEG C, and reaction point pressure-controlled is at 1KPa, and the reaction times controls at 1h.During reaction, porous carbon template is placed in Si and SiO
2above mixed powder, and porous carbon template and reaction vessel inwall close contact, reactant gases is conducive to porous carbon template internal diffusion.
The present embodiment gained C/SiC porous composite ceramics performance sees attached list 1.
Embodiment 2:
Step 1: choosing density is 0.6g/cm
3chopped carbon fiber prefabricated component as skeleton; Using sucrose as carbon source, compound concentration is the sucrose solution of 70g/L;
Step 2: adopt microwave hydrothermal technology, sucrose solution and carbon fiber skeleton are put into micro-wave diminishing pot, and then micro-wave diminishing pot is put into microwave attenuation materials instrument and react, obtain the carbon fiber skeleton that carbosphere bonds.Temperature of reaction controls at 210 DEG C, and the reaction times controls at 1.5h, and final carbosphere is of a size of 500nm.
Step 3: the porous carbon template after step 4 being processed, puts into vacuum sintering furnace.With Si and SiO
2mixed powder as silicon source, Si:SiO
2mol ratio controls at 2:3, and temperature of reaction controls at 1600 DEG C, and reaction point pressure-controlled is at 100KPa, and the reaction times controls at 4h.During reaction, porous carbon template is placed in Si and SiO
2above mixed powder, and porous carbon template and reaction vessel inwall close contact, reactant gases is conducive to porous carbon template internal diffusion.
The present embodiment gained C/SiC porous composite ceramics performance sees attached list 1.
Embodiment 3:
Step 1: choosing density is 0.4g/cm
3chopped carbon fiber prefabricated component as skeleton; Using starch as carbon source, compound concentration is the starch solution of 30g/L;
Step 2: adopt microwave hydrothermal technology, starch solution and carbon fiber skeleton are put into micro-wave diminishing pot, and then micro-wave diminishing pot is put into microwave attenuation materials instrument and react, obtain the carbon fiber skeleton that carbosphere bonds.Temperature of reaction controls at 200 DEG C, and the reaction times controls at 2h, and final carbosphere is of a size of 300nm.
Step 3: the porous carbon template after step 4 being processed, puts into vacuum sintering furnace.With Si and SiO
2mixed powder as silicon source, Si:SiO
2mol ratio controls at 1:1, and temperature of reaction controls at 1500 DEG C, and reaction point pressure-controlled is at 10KPa, and the reaction times controls at 2h.During reaction, porous carbon template is placed in Si and SiO
2above mixed powder, and porous carbon template and reaction vessel inwall close contact, reactant gases is conducive to porous carbon template internal diffusion.
The present embodiment gained C/SiC porous composite ceramics performance sees attached list 1.
Embodiment 4:
Step 1: choosing density is 0.5g/cm
3chopped carbon fiber prefabricated component as skeleton; Using glucose as carbon source, compound concentration is the glucose solution of 100g/L;
Step 2: adopt microwave hydrothermal technology, glucose solution and carbon fiber skeleton are put into micro-wave diminishing pot, and then micro-wave diminishing pot is put into microwave attenuation materials instrument and react, obtain the carbon fiber skeleton that carbosphere bonds.Temperature of reaction controls at 190 DEG C, and the reaction times controls at 2.5h, and final carbosphere is of a size of 400nm.
Step 3: the porous carbon template after step 4 being processed, puts into vacuum sintering furnace.With Si and SiO
2mixed powder as silicon source, Si:SiO
2mol ratio controls at 2:1, and temperature of reaction controls at 1400 DEG C, and reaction point pressure-controlled is at 50KPa.Reaction times is 3h, and porous carbon template is placed in Si and SiO
2above mixed powder, and porous carbon template and reaction vessel inwall close contact, reactant gases is conducive to porous carbon template internal diffusion.
The present embodiment gained C/SiC porous composite ceramics performance sees attached list 1.
Embodiment 5:
Step 1: choosing density is 0.3g/cm
3chopped carbon fiber prefabricated component as skeleton; Using sucrose as carbon source, compound concentration is the sucrose solution of 10g/L;
Step 2: adopt microwave hydrothermal technology, sucrose solution and carbon fiber skeleton are put into micro-wave diminishing pot, and then micro-wave diminishing pot is put into microwave attenuation materials instrument and react, obtain the carbon fiber skeleton that carbosphere bonds.Temperature of reaction controls at 180 DEG C, and the reaction times controls at 3h, and final carbosphere is of a size of 300nm.
Step 5: the porous carbon template after step 2 being processed, puts into vacuum sintering furnace.With Si and SiO
2mixed powder as silicon source, Si:SiO
2mol ratio controls at 1:1, and temperature of reaction controls at 1300 DEG C, and reaction point pressure-controlled is at 30KPa, and the reaction times is 2h.During reaction, porous carbon template is placed in Si and SiO
2above mixed powder, and porous carbon template and reaction vessel inwall close contact, reactant gases is conducive to porous carbon template internal diffusion.
The present embodiment gained C/SiC porous composite ceramics performance sees attached list 1.
The specific surface area of subordinate list 1.C/SiC porous composite ceramics sample and ultimate compression strength index
With reference to shown in Fig. 2, it is scanning electron microscope (SEM) photo of the C/SiC porous composite ceramics that the present embodiment 4 obtains.As can be seen from Fig. 2 (a): after microwave hydrothermal process, carbon fiber surface deposits one deck carbon and a large amount of carbosphere of surface arrangement; Fig. 2 (b) reacts the SiC layer and SiC microballoon (micro-prominent) generated for carbothermic reduction reaction process carbon fiber surface carbon-coating and carbosphere and gas phase SiO, can find out, SiC layer has uneven surface, be made up of a large amount of nano SiC granule, this is that the high-specific surface area of porous composite ceramics provides powerful guarantee; And the formation of the SiC microballoon heredity microscopic appearance of carbosphere; As can be seen from corresponding enlarged view 2 (c): single SiC microsphere surface is coarse, is made up of nano SiC granule.Fig. 2 (d) radially distributes in SiC microsphere surface for the SiC nanowire (fine hair) on the micro-prominent surface of SiC when the reaction times is 1h, nano wire.Fig. 2 (e) is the SiC nanowire (fine hair) on the micro-prominent surface of SiC when the reaction times is 3h, along with the reaction times extends, SiC nanowire length-to-diameter ratio increases, and is distributed in porous composite ceramics hole, further increases the specific surface area of porous composite ceramics.
The method that preparation provided by the invention has biomimetic features C/SiC porous composite ceramics at least has the following advantages: the present invention chooses chopped carbon fiber prefabricated component as skeleton, microwave-hydrothermal method is adopted to build carbon fiber skeleton structure at carbon fiber surface deposit carbon microballoon, form the three-dimensional net structure of a high porosity, high strength, in conjunction with the feature of carbon fiber high-strength light, it is the basis of C/SiC porous composite ceramics; Utilize carbothermic reduction reaction that carbon fiber surface carbosphere and gas phase SiO are reacted and generate SiC, SiC layer and the SiC microsphere surface of carbon fiber surface are coarse, are made up of a large amount of nano SiC granule; And hereditary carbosphere microtexture, form SiC at carbon fiber surface micro-prominent, this is that the high-specific surface area of porous composite ceramics provides powerful guarantee; Utilize gas phase SiO and CO to react and form SiC nanometer fine hair (SiC nanowire) on the micro-prominent surface of SiC, construct and there is biomimetic features C/SiC porous composite ceramics.SiC nanowire is distributed in porous composite ceramics hole, further increases the specific surface area of porous composite ceramics.The structure of this biomimetic features, significantly can improve the specific surface area of SiC porous ceramics, makes it have potential application at catalyst support material and high temperature air filtration field.
Feature of the present invention comprise following some:
1:C/SiC porous composite ceramics is by carbon fiber as skeleton, and carbon fiber skeleton can derive from chopped carbon fiber prefabricated component, carbon fiber stereo fabric.
2: by microwave hydrothermal technology, prepare carbosphere on the surface of carbon fiber, carbon fiber is connected as a whole, the intensity of enhanced carbon fiber skeleton.The carbosphere simultaneously prepared can protect carbon fiber as carbon source in follow-up carbothermic reduction reaction.
3: in carbon fiber skeleton, introducing carbosphere is the preparation micro-prominent basis of SiC.The microtexture that the micro-prominent formation of SiC has been hereditary carbosphere is the basis of C/SiC porous composite ceramics high-specific surface area.
4: on the micro-prominent surface of SiC, be distributed with a large amount of SiC nanometer fine hair (SiC nanowire).The existence of a large amount of SiC nanometer fine hair, significantly can improve the specific surface area of porous composite ceramics, makes it have potential application at catalyst support material and high temperature air filtration field.
Claims (10)
1. one kind has the preparation method of biomimetic features C/SiC porous composite ceramics, it is characterized in that: having biomimetic features C/SiC porous composite ceramics take carbon fiber as skeleton, adopt microwave-hydrothermal method at carbon fiber surface deposit carbon microballoon, to build carbon fiber network skeleton, then, carbothermic reduction reaction is utilized to form SiC at carbon fiber surface micro-prominent, then, form SiC nanometer fine hair on the micro-prominent surface of SiC, thus construct there is biomimetic features C/SiC porous composite ceramics.
2. a kind of preparation method with biomimetic features C/SiC porous composite ceramics according to claim 1, it is characterized in that: the formation method of the carbosphere of described carbon fiber surface is: take carbon fiber as skeleton, take glucose as carbon source, skeleton and carbon source are positioned in micro-wave diminishing pot, again micro-wave diminishing pot is put into microwave attenuation materials instrument to react, temperature of reaction is 170 ~ 210 DEG C, and the reaction times is 1 ~ 3h.
3. a kind of preparation method with biomimetic features C/SiC porous composite ceramics according to claim 2, is characterized in that: the concentration of described glucose solution is 10 ~ 100g/L.
4. a kind of preparation method with biomimetic features C/SiC porous composite ceramics according to claim 1, it is characterized in that: micro-the dashing forward of described SiC utilizes carbothermic reduction reaction that carbon fiber surface carbosphere and gas phase SiO are reacted to generate SiC, and hereditary carbosphere microtexture, form SiC at carbon fiber surface micro-prominent.
5. a kind of preparation method with biomimetic features C/SiC porous composite ceramics according to claim 1 or 4, is characterized in that: described SiC nanometer fine hair utilizes gas phase SiO and CO to react to be formed on the micro-prominent surface of SiC.
6. there is a preparation method for biomimetic features C/SiC porous composite ceramics, it is characterized in that: comprise the following steps:
Step 1: take carbon fiber as skeleton, take glucose as carbon source, adopt microwave hydrothermal technology, glucose solution and carbon fiber skeleton are put into micro-wave diminishing pot, and then micro-wave diminishing pot is put into microwave attenuation materials instrument react, obtain the carbon fiber skeleton of carbosphere bonding;
Step 2: carbon fiber skeleton step 1 obtained puts into vacuum sintering furnace, with Si and SiO
2mixed powder is as silicon source, and controlling temperature of reaction is 1300 ~ 1600 DEG C, and reaction pressure is 1 ~ 100KPa, and the reaction times is 1 ~ 4h.
7. a kind of preparation method with biomimetic features C/SiC porous composite ceramics according to claim 6, it is characterized in that: in described step 2, carbon fiber skeleton is placed in Si and SiO
2above mixed powder.
8. a kind of preparation method with biomimetic features C/SiC porous composite ceramics according to claim 6, is characterized in that: the inwall close contact of described carbon fiber skeleton and sintering oven, makes reactant gases be conducive to spreading to carbon fiber skeletal internal.
9. one kind has biomimetic features C/SiC porous composite ceramics based on the one in claim 1 to 8 prepared by any one method.
10. one kind has biomimetic features C/SiC porous composite ceramics, it is characterized in that: this composite ceramics comprises carbon fiber, the carbosphere utilizing microwave hydrothermal to react formation between carbon fiber connects, carbon fiber and carbosphere are built into carbon fiber network skeleton, it is micro-prominent that described carbosphere utilizes carbothermic reduction reaction to form SiC at carbon fiber surface, is formed with SiC nanometer fine hair micro-the dashing forward of this SiC.
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| CN114436674A (en) * | 2022-02-11 | 2022-05-06 | 洛阳理工学院 | Preparation method of network-like silicon carbide fiber |
| CN114436674B (en) * | 2022-02-11 | 2023-04-11 | 洛阳理工学院 | Preparation method of network-like silicon carbide fiber |
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