CN104817337B - A kind of porous composite ceramicses of Multi-scale model SiC/C and preparation method thereof - Google Patents
A kind of porous composite ceramicses of Multi-scale model SiC/C and preparation method thereof Download PDFInfo
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Abstract
A kind of porous composite ceramicses of Multi-scale model SiC/C and preparation method thereof; skeleton is used as using Polyacrylonitrile carbon fiber felt; by hydrothermal carbonization technology in Polyacrylonitrile carbon fiber felt surface deposited carbon layer; recycle carbothermic reduction reaction to grow SiC protective layers and SiC nanowire in skeleton, obtain the porous composite ceramicses of Multi-scale model SiC/C.The present invention is by hydrothermal carbonization technology in carbon fiber surface deposited carbon layer, carbon fiber is connected into a porous carbon skeleton, the intensity and specific surface area of carbon skeleton can be improved, then using CO as carbon source, SiO is used as silicon source, using chemical gas-phase reaction method, SiC layer and SiC nanowire are generated in carbon skeleton, a porous composite ceramics of SiC/C is built, the porous composite ceramicses of SiC/C produced by the present invention not only have high-specific surface area, and with easy-formation, the characteristics of high intensity.
Description
Technical field
The invention belongs to porous ceramic film material preparing technical field, it is related to a kind of porous composite ceramics of Multi-scale model SiC/C
Porcelain and preparation method thereof.
Background technology
SiC is the covalent key compound being made up of carbon and silicon, and the tetrahedral structural unit with class dimantine not only has
Have extraordinary chemical stability, high mechanical strength and hardness, and with good thermal conductivity.Especially SiC
Good electrical and thermal conductivity is conducive between catalyst heat transfer during the course of the reaction and catalyst activity component and carrier
Electron transmission, carborundum turns into the ideal material of catalyst carrier.But, but seldom see in chemical industry catalysis technical field
The figure of SiC porous ceramics application.To find out its cause, be because the SiC porous ceramics produced of commercial methods its compare surface
Product is difficult to the requirement for meeting catalyst carrier material.Therefore, the high-specific surface area carbonization that can serve as catalyst carrier how is prepared
Silicon, has caused the attention of researcher, and relevant research is also increasing, develops template, sol-gal process, Polycarbosilane
The methods such as cracking process, are prepared for SiC porous particles, SiC nanotubes, the structure such as SiC microballoons.
Chinese invention patent 02130064.X reports a kind of high-specific surface area carborundum and preparation method thereof, this method institute
A diameter of 10-20nm of the high-specific surface area carborundum of preparation, specific surface area is 60-160m2/ g, pore size distribution range is 3-
100nm.However, high-specific surface area SiC prepared by the above method will reach that practical application also needs shaping, carry the catalyst being made
Body has suitable shape, size and mechanical strength, to meet the operation requirement of industrial reactor.In the process of shaping of catalyst
In, the sintering process of porous SiC ceramics can cause being greatly reduced for specific surface area.Therefore, a kind of carbon of high-specific surface area is developed
SiClx porous ceramics and preparation method thereof is also strong with stronger formability and machinery while making it have specific area
Degree is to solve the key that the material is applied in catalytic field.
The content of the invention
Multi-scale model SiC/C porous ceramics and preparation method thereof is prepared it is an object of the invention to provide one kind, is made
The characteristics of SiC/C porous ceramics has high-specific surface area, high intensity, high porosity.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of the porous composite ceramicses of Multi-scale model SiC/C, bone is used as using Polyacrylonitrile carbon fiber felt
Frame, by hydrothermal carbonization technology in Polyacrylonitrile carbon fiber felt surface deposited carbon layer, recycles carbothermic reduction reaction in skeleton
Interior growth SiC protective layers and SiC nanowire, obtain the porous composite ceramicses of Multi-scale model SiC/C.
Specifically include following steps：
Step 1：Polyacrylonitrile carbon fiber felt as skeleton is put into hydrothermal reaction kettle, then added as carbon source
The sucrose solution of presoma, at 180 DEG C~250 DEG C of reaction temperature, deposition is after 2~8 hours by Polyacrylonitrile carbon fiber felt
Take out, drying；
Step 2：By Si and SiO2Mixed-powder, step 1 dry Polyacrylonitrile carbon fiber felt be put into graphite crucible
In, then graphite crucible is put into vacuum sintering furnace, is passed through when temperature rises to 1200 DEG C~1500 DEG C into graphite crucible
CO gases are sintered, and room temperature is then down to naturally, obtain the porous composite ceramicses of Multi-scale model SiC/C.
The density of the Polyacrylonitrile carbon fiber felt is 0.2~0.6g/cm3。
The concentration of the sucrose solution is 100g~500g/L.
The ratio of sucrose is (1~5) g in the Polyacrylonitrile carbon fiber felt and sucrose solution：(30~50) mL.
The bottom belt of the graphite crucible has the breather pipe for being passed through gas into crucible and extending into inside crucible,
Si and SiO2The height of mixed-powder be less than the height of breather pipe extending into inside crucible, the polyacrylonitrile that step 1 is dried
Base carbon fibre felt is positioned at the opening of graphite crucible.
The flow of the CO gases is 1L~10L/h.
Si and SiO in the step 22Mixed-powder in Si and SiO2Mol ratio be 1:1~2:1.
Sintering time for 1~3 hour in the step 2.
A kind of porous composite ceramicses of the SiC/C of Multi-scale model, the specific surface areas of the porous composite ceramicses of the SiC/C for 80~
110m2/ g, pore size distribution range is 0.3~100 μm, and intensity is 13~22MPa, and porosity is 65~87%.
Compared with prior art, the device have the advantages that：The present invention is used as carbon using Polyacrylonitrile carbon fiber felt
Skeleton, by hydrothermal carbonization technology in carbon fiber surface deposited carbon layer, a porous carbon skeleton, Neng Gouti are connected into by carbon fiber
The intensity and specific surface area of high carbon skeleton, then using CO as carbon source, SiO is as silicon source, using chemical gas-phase reaction method 1200
In~1500 DEG C of temperature ranges, SiC layer and SiC nanowire are generated in carbon skeleton, a porous composite ceramics of SiC/C is built,
The porous composite ceramicses of the SiC/C are combined by carbon fiber, carbosphere, SiC layer, SiC nanowire, are a micro-nano multistage knots
The porous composite ceramics of structure, and the porous composite ceramicses of SiC/C produced by the present invention not only have high-specific surface area, and have
The characteristics of easy-formation, high intensity, its compression strength may be up to 22MPa.The porous composite ceramicses of SiC/C produced by the present invention can be straight
Connect as catalyst carrier, it is not necessary to will can meet the behaviour of industrial reactor after the SiC shapings of obtained high-specific surface area
Need, so saving operating procedure using the porous composite ceramicses of SiC/C produced by the present invention, reduce cost, and keep away
Exempt to cause the problem of specific surface area is reduced in SiC forming processes.
The method that the present invention prepares the porous composite ceramicses of SiC/C has further the advantage that：It is fine with polyacrylonitrile-based carbon first
Felt is tieed up as skeleton, the characteristics of forming high porosity, a three-dimensional net structure for high intensity, carbon fiber high-strength light is
The basis of the porous composite ceramicses of SiC/C, then using hydrothermal carbonization method on carbon fiber skeleton deposited carbon layer, carbon can be connected fine
Skeleton is tieed up, the intensity of carbon fiber skeleton is improved, the ratio of carbon skeleton can be also greatly improved in the carbosphere of hydrothermal carbonization generation
Surface area.
Further, the present invention is first fine in the polyacrylonitrile-based carbon as skeleton using sucrose solution as carbon source presoma
Deposited carbon layer on felt is tieed up, carbon source, Si and SiO are then used as using CO2The SiO of reaction generation reacts as silicon source in carbon skeleton
SiC is deposited, this method has the characteristics of cost is low, and CO and SiO reaction system is more easy to grow SiC in stephanoporate framework and received
Rice noodles, constitute a porous composite ceramics of SiC/C with micro-nano multilevel hierarchy, and intensity is 13~22MPa.
Further, because the bottom belt of graphite crucible has for being passed through gas into crucible and extending into the present invention
Breather pipe inside crucible, Si and SiO2The height of mixed-powder be less than the height of breather pipe extending into inside crucible, dry
Dry Polyacrylonitrile carbon fiber felt is positioned at the opening of graphite crucible, and such location layout, which to work as, reaches reaction temperature
When, the CO gases being passed through into crucible can be good at and Si and SiO2The SiO reactions of reaction generation, are generated in carbon skeleton
SiC layer and SiC nanowire, so as to obtain the SiC/C porous ceramics of Multi-scale model.
Further, due to CO gases be as carbon source, so its flow be 1L~10L/h just can guarantee that SiC layer and
The generation of SiC nanowire.
The specific surface area of the porous composite ceramicses of SiC/C produced by the present invention is 80~110m2/ g, pore size distribution range is
0.3~100 μm, intensity is 13~22MPa, and porosity is 65~87%.
Brief description of the drawings
Fig. 1 is the schematic device for preparing the porous composite ceramicses of SiC/C of the present invention；
Fig. 2 is the low power microscopic appearance figure of the porous composite ceramicses of SiC/C of the present invention；
Fig. 3 is the high power micro-structure diagram of the porous composite ceramicses of SiC/C of the present invention.
In figure, 1 is graphite crucible, and 2 be breather pipe, and 3 be Si and SiO2Mixed-powder, 4 be carbon fiber skeleton.
Embodiment
The present invention is using Polyacrylonitrile carbon fiber felt as skeleton, by hydrothermal carbonization technology in polyacrylonitrile-based carbon fibre
Felt surface deposited carbon layer, recycles carbothermic reduction reaction to grow SiC protective layers and SiC nanowire in skeleton, obtains multiple dimensioned
The porous composite ceramicses of structure SIC/C.
Specific preparation process is as follows：
Step 1：Selection density is 0.2~0.6g/cm3Polyacrylonitrile carbon fiber felt be used as carbon fiber skeleton；Will choosing
The carbon fiber skeleton taken is put into hydrothermal reaction kettle, using sucrose solution as carbon source presoma, reaction temperature be 180 DEG C~
At 250 DEG C, sedimentation time is to take out Polyacrylonitrile carbon fiber felt carbon skeleton after 2~8 hours, is dried；Wherein, sucrose solution
Concentration is controlled in 100g~500g/L, and the ratio of Polyacrylonitrile carbon fiber felt and sucrose solution is (1~5) g：(30~50) mL.
Step 2：By Si and SiO2Mixed-powder 3, by step 1 drying after carbon fiber skeleton 4 be added to graphite earthenware
In crucible 1, the bottom belt of graphite crucible 1 has a breather pipe 2 for being passed through gas into crucible and extending into inside crucible, Si with
SiO2The height of mixed-powder be less than the height of graphite breather pipe 2 extending into inside crucible, the carbon fiber bone that step 1 is dried
Frame 4 is positioned at the opening of graphite crucible 1, and the top of the lower surface of carbon fiber skeleton 4 and the breather pipe extending into inside crucible
There is interval (referring to Fig. 1) at end, then graphite crucible 1 is put into vacuum sintering furnace, when temperature rises to 1200 DEG C~1500 DEG C
CO gases are passed through into graphite crucible 1 by breather pipe 2, after reacting 1~3 hour, room temperature is down to naturally, carbon fiber bone is taken out
Frame, that is, obtain the porous composite ceramicses of Multi-scale model SiC/C；Wherein, Si and SiO2Mixed-powder in Si:SiO2Mol ratio control
System is 1:1~2:1, CO gas flow is controlled in 1L~10L/h.
Polyacrylonitrile carbon fiber felt, Si and SiO in above-mentioned graphite crucible2Mixed-powder and with extending into graphite earthenware
The setting of breather pipe position in crucible, ensure that Si and SiO2The gaseous state silicon monoxide of generation is reacted as silicon source and is used as carbon
The CO gases in source SiC layer and SiC nanowire in carbon fiber skeleton, are combined beneficial to finally having the porous of micro-nano multilevel hierarchy
The formation of ceramics.
The inventive method is further elaborated with reference to specific embodiment, in the graphite crucible in embodiment 1-5
Si and SiO2Mixed-powder 3, the position relationship of carbon fiber skeleton 4 and the breather pipe extending into graphite crucible referring to Fig. 1,
The bottom belt of graphite crucible 1 has the breather pipe 2 for being passed through gas into crucible and extending into inside crucible, Si and SiO2's
The height of mixed-powder 3 is less than the height of the breather pipe inside crucible, and the carbon fiber estimation that step 1 is dried is positioned over graphite crucible
Opening at, the mouth of graphite crucible 1 is sealed, and there are interval, i.e. graphite in the lower surface of carbon fiber skeleton 4 and the top of breather pipe
The Si and SiO of the inner bottom part of crucible 12Mixed-powder 3 and top carbon fiber skeleton 4 between form cavity, the outlet of breather pipe 2
In cavity.
Embodiment 1
Step 1：Selection density is 0.2g/cm3Polyacrylonitrile carbon fiber felt be used as carbon fiber skeleton；
Step 2：The carbon fiber skeleton that step 1 is chosen is put into hydrothermal reaction kettle, is then added as carbon source presoma
Sucrose solution, reaction temperature be 180 DEG C at, deposition 2 hours after carbon fiber skeleton is taken out, dry；Wherein, sucrose solution
Concentration be 100g/L, the ratio of Polyacrylonitrile carbon fiber felt and sucrose solution is 1g：30mL.
Step 3：By Si and SiO2Carbon fiber skeleton after mixed-powder, step 2 drying is added in graphite crucible, then
Graphite crucible is put into vacuum sintering furnace, when temperature rises to 1200 DEG C, is passed through by graphite breather pipe into graphite crucible
CO gases are sintered 1 hour, are then naturally cooling to obtain the porous composite ceramicses of Multi-scale model SiC/C after room temperature；Wherein,
Si and SiO2Si in mixed-powder:SiO2Mol ratio is 2:1, CO gas flow is 1L/h.
The specific surface area of the porous composite ceramicses of SiC/C obtained by the present embodiment is 80m2/g；Pore size distribution range is 0.3
~100 μm, the aperture of wherein 0.3-4 μ ms accounts for 8% (percent by volume), and the aperture of 4-50 μ ms accounts for 15% (body
Product percentage)；Intensity is 13MPa；Porosity is 65%.
Embodiment 2
Step 1：Selection density is 0.6g/cm3Polyacrylonitrile carbon fiber felt be used as carbon fiber skeleton；
Step 2：The carbon fiber skeleton that step 1 is chosen is put into hydrothermal reaction kettle, is then added as carbon source presoma
Sucrose solution, reaction temperature be 250 DEG C at, deposition 8 hours after carbon fiber skeleton is taken out, dry.Wherein, sucrose solution
Concentration be 500g/L, the ratio of Polyacrylonitrile carbon fiber felt and sucrose solution is 2g：45mL.
Step 3：By Si and SiO2Carbon fiber skeleton after mixed-powder, step 2 drying is added in graphite crucible, then
Graphite crucible is put into vacuum sintering furnace, when temperature rises to 1500 DEG C, is passed through by graphite breather pipe into graphite crucible
CO gases are sintered 3 hours, are then naturally cooling to obtain the porous composite ceramicses of Multi-scale model SiC/C after room temperature；Wherein,
Si and SiO2Si in mixed-powder:SiO2Mol ratio is 1:1, CO gas flow is 10L/h.
The specific surface area of the porous composite ceramicses of SiC/C obtained by the present embodiment is 87m2/g；Pore size distribution range is 0.3
~100 μm, the aperture of wherein 0.3-4 μ ms accounts for 10% (percent by volume), and the aperture of 4-50 μ ms accounts for 13% (body
Product percentage)；Intensity is 15MPa；Porosity is 70%.
Embodiment 3
Step 1：Selection density is 0.3g/cm3Polyacrylonitrile carbon fiber felt be used as carbon fiber skeleton；
Step 2：The carbon fiber skeleton that step 1 is chosen is put into hydrothermal reaction kettle, is then added as carbon source presoma
Sucrose solution, reaction temperature be 200 DEG C at, deposition 4 hours after carbon fiber skeleton is taken out, dry；Wherein sucrose solution
Concentration be 200g/L, the ratio of Polyacrylonitrile carbon fiber felt and sucrose solution is 5g：50mL.
Step 3：By Si and SiO2Carbon fiber skeleton after mixed-powder, step 2 drying is added in graphite crucible, then
Graphite crucible is put into vacuum sintering furnace, when temperature rises to 1300 DEG C, is passed through by graphite breather pipe into graphite crucible
CO gases are sintered 1.5 hours, are then naturally cooling to obtain the porous composite ceramicses of Multi-scale model SiC/C after room temperature；Its
In, Si and SiO2Si in mixed-powder:SiO2Mol ratio is 1.3:1, CO gas flow is 3L/h.
The specific surface area of the porous composite ceramicses of SiC/C obtained by the present embodiment is 95m2/g；Pore size distribution range is 0.3
~100 μm, the aperture of wherein 0.3-4 μ ms accounts for 12% (percent by volume), and the aperture of 4-50 μ ms accounts for 15% (body
Product percentage)；Intensity is 17MPa；Porosity is 75%.
Embodiment 4
Step 1：Selection density is 0.4g/cm3Polyacrylonitrile carbon fiber felt be used as carbon fiber skeleton；
Step 2：The carbon fiber skeleton that step 1 is chosen is put into hydrothermal reaction kettle, is then used as carbon source forerunner to add
The sucrose solution of body, in the case where reaction temperature is 220 DEG C, deposition took out carbon fiber skeleton after 5 hours, dried；Wherein, sucrose is molten
The concentration of liquid is 300g/L, and the ratio of Polyacrylonitrile carbon fiber felt and sucrose solution is 4g：35mL.
Step 3：By Si and SiO2Carbon fiber skeleton after mixed-powder, step 2 drying is added in graphite crucible, then
Graphite crucible is put into vacuum sintering furnace, when temperature rise to after 1400 DEG C begin through graphite breather pipe into graphite crucible lead to
Enter CO gases to be sintered 2.5 hours, be then naturally cooling to obtain the porous composite ceramicses of Multi-scale model SiC/C after room temperature；
Wherein, Si and SiO2Si in mixed-powder:SiO2Mol ratio is 1.6:1, CO gas flow is 5L/h.
Fig. 2 and Fig. 3 is ESEM (SEM) photo of SiC/C porous ceramics made from the present embodiment 4.It can be seen by Fig. 2
Go out：Carbon fiber is in three-dimensional netted distribution, the substantial amounts of SiC nanowire of superficial growth；It can be seen that by corresponding enlarged drawing 3：Carbon fiber
There is a SiC layer on surface, is made up of a large amount of SiC micro-nano granules.SiC nanowire is filled with the hole between carbon fiber.This implementation
The specific surface area of the porous composite ceramicses of SiC/C obtained by example is 110m2/g；Pore size distribution range is 0.3~100 μm, wherein
The aperture of 0.3-4 μ ms accounts for 15% (percent by volume), and the aperture of 4-50 μ ms accounts for 20% (percent by volume)；By force
Spend for 20MPa；Porosity is 80%.
Embodiment 5
Step 1：Selection density is 0.5g/cm3Polyacrylonitrile carbon fiber felt be used as carbon fiber skeleton；
Step 2：The carbon fiber skeleton that step 1 is chosen is put into hydrothermal reaction kettle, is then added as carbon source presoma
Sucrose solution, reaction temperature be 240 DEG C at, deposition 3 hours after carbon fiber skeleton is taken out, dry.Wherein, sucrose solution
Concentration be 350g/L, the ratio of Polyacrylonitrile carbon fiber felt and sucrose solution is 5g：40mL.
Step 3：By Si and SiO2Carbon skeleton after mixed-powder, step 2 drying is added in graphite crucible, then by stone
Black crucible is put into vacuum sintering furnace, and 2 are sintered when temperature rises to after 1450 DEG C to start to be passed through CO gases into graphite crucible
Hour, then it is naturally cooling to obtain the porous composite ceramicses of Multi-scale model SiC/C after room temperature；Wherein, Si and SiO2Mixed powder
Si in end:SiO2Mol ratio is 1.8:1, CO gas flow is 8L/h.
The specific surface area of the porous composite ceramicses of SiC/C obtained by the present embodiment is 103m2/g；Pore size distribution range is
0.3~100 μm, the aperture of wherein 0.3-4 μ ms accounts for 13% (percent by volume), and the aperture of 4-50 μ ms accounts for 17%
(percent by volume)；Intensity is 22MPa；Porosity is 87%.
The present invention deposits carbon by hydrothermal carbonization technology using Polyacrylonitrile carbon fiber felt as skeleton in carbon fiber surface
Layer, to improve the intensity and specific surface area of carbon skeleton, then using CO as carbon source, SiO is existed as silicon source using carbothermic reduction reaction
Growth SiC protective layers and SiC nanowire in carbon skeleton, build a porous composite ceramics of SiC/C.The porous composite ceramics of the SiC/C
Porcelain is combined by carbon fiber, carbosphere, SiC layer, SiC nanowire, is the porous composite ceramic of a micro-nano Multi-scale model
Porcelain.Carbon fiber is connected into a porous carbon skeleton, energy by carbon fiber skeleton by hydrothermal carbonization method deposited carbon layer in the present invention
Enough improve the intensity and specific surface area of carbon skeleton.SiC is deposited in carbon stephanoporate framework and the method for growth SiC nanowire is specially
Chemical gas-phase reaction method：Using CO as carbon source, SiO is as silicon source, the reaction generation SiC layer in 1200~1500 DEG C of temperature ranges
And SiC nanowire；Carbon source in hydrothermal carbonization method is sucrose solution, and the concentration of sucrose solution is 100g~500g/L, is sunk
Accumulated temperature degree is at 180 DEG C~250 DEG C, and sedimentation time was at 2~8 hours.
Claims (7)
1. a kind of preparation method of the porous composite ceramicses of Multi-scale model SiC/C, it is characterised in that with polyacrylonitrile-based carbon fibre
Felt is as skeleton, by hydrothermal carbonization technology in Polyacrylonitrile carbon fiber felt surface deposited carbon layer, recycles carbon thermal reduction anti-
SiC protective layers and SiC nanowire should be grown in skeleton, the porous composite ceramicses of Multi-scale model SiC/C are obtained；
Specifically include following steps：
Step 1：Polyacrylonitrile carbon fiber felt as skeleton is put into hydrothermal reaction kettle, then added as carbon source forerunner
The sucrose solution of body, at 180 DEG C~250 DEG C of reaction temperature, deposition took out Polyacrylonitrile carbon fiber felt after 2~8 hours,
Drying；
Step 2：By Si and SiO2Mixed-powder, step 1 dry Polyacrylonitrile carbon fiber felt be put into graphite crucible, so
Graphite crucible is put into vacuum sintering furnace afterwards, CO gases are passed through into graphite crucible when temperature rises to 1200 DEG C~1500 DEG C
It is sintered, room temperature is then down to naturally, obtains the porous composite ceramicses of Multi-scale model SiC/C；
The flow of the CO gases is 1L~10L/h；
The bottom belt of graphite crucible has the breather pipe for being passed through gas into crucible and extending into inside crucible, Si and SiO2
Mixed-powder height of the height less than the breather pipe inside crucible, the carbon fiber that step 1 is dried is positioned over graphite crucible
At opening, the mouth of graphite crucible is sealed, and there is an interval on the lower surface of carbon fiber skeleton and the top of breather pipe, breather pipe goes out
Mouth is located in graphite crucible cavity.
2. a kind of preparation method of porous composite ceramicses of Multi-scale model SiC/C according to claim 1, its feature exists
In the density of the Polyacrylonitrile carbon fiber felt is 0.2~0.6g/cm3。
3. a kind of preparation method of porous composite ceramicses of Multi-scale model SiC/C according to claim 1, its feature exists
In the concentration of the sucrose solution is 100g~500g/L.
4. a kind of preparation method of porous composite ceramicses of Multi-scale model SiC/C according to claim 3, its feature exists
In the ratio of the Polyacrylonitrile carbon fiber felt and sucrose solution is (1~5) g：(30~50) mL.
5. a kind of preparation method of porous composite ceramicses of Multi-scale model SiC/C according to claim 1, its feature exists
In Si and SiO in the step 22Mixed-powder in Si and SiO2Mol ratio be 1:1~2:1.
6. a kind of preparation method of porous composite ceramicses of Multi-scale model SiC/C according to claim 1, its feature exists
In the time sintered in the step 2 is 1~3 hour.
7. a kind of porous composite ceramicses of SiC/C of Multi-scale model prepared by method according to claim 1, its feature exists
In the specific surface area of the porous composite ceramicses of the SiC/C is 80~110m2/ g, pore size distribution range is 0.3~100 μm, and intensity is
13~22MPa, porosity is 65~87%.
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| CN105622172B (en) * | 2015-12-25 | 2018-08-24 | 中国科学院上海硅酸盐研究所 | The fiber surface of non-oxidized substance fiber reinforced ceramic matrix composites is prepared in situ (C-SiC)nOr the method for SiC coatings |
| CN107188527B (en) * | 2017-06-19 | 2019-10-11 | 西安交通大学 | A kind of SiC flexible ceramic and preparation method thereof constructed by nano wire |
| CN107456945B (en) * | 2017-07-03 | 2020-05-19 | 柏美迪康环境工程（上海）股份有限公司 | Modified carbonaceous adsorbent and preparation and application methods thereof |
| CN107512780B (en) * | 2017-09-29 | 2020-11-10 | 福建省农业科学院农业工程技术研究所 | Bacterial carbon water purifying agent for removing high-concentration ammonia nitrogen in aquaculture sewage and preparation method thereof |
| CN108004767B (en) * | 2017-12-06 | 2020-03-10 | 中国科学院宁波材料技术与工程研究所 | Method for preparing hydrothermal carbon layer on surface of carbon fiber and application of hydrothermal carbon layer |
| US20220008882A1 (en) * | 2018-10-29 | 2022-01-13 | China Petroleum & Chemical Corporation | Porous Composite Material Capable of Generating Electric Arc in Microwave Field, Preparation Method therefor, and Use thereof |
| CN112030544B (en) * | 2020-08-31 | 2021-06-15 | 北京航空航天大学 | Method for in-situ growth of silicon carbide nanowires on surface of silicon carbide fiber |
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