CN107188527A - A kind of SiC flexible ceramics constructed by nano wire and preparation method thereof - Google Patents
A kind of SiC flexible ceramics constructed by nano wire and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of SiC flexible ceramics constructed by nano wire and preparation method thereof, belong to advanced ceramics preparing technical field.Technical scheme is：Using porous carbon materials or porous carbon fiber material as skeleton, the polysiloxanes colloidal sol prepared is hydrolyzed as presoma using alkoxy silane, pass through infiltration pyrolysis gas phase reaction, obtain porous carbon materials or porous carbon fiber material/SiC nanowire intermediate structure, then porous carbon materials or porous carbon fiber material skeleton are removed by thermal oxide, obtains the SiC flexible ceramics that nano wire is constructed.The material be by SiC nanowire by be self-assembly of have some strength, good elastoplasticity, excellent thermal insulation performance lightweight three-dimensional net structure.To prepare the new method of flexible ceramic large scale, the preparation of complex-shaped SiC flexible ceramics can be achieved, while short preparation period, cost is low, suitable for industrialized production in this method.
Description
Technical field
The invention belongs to advanced ceramics preparing technical field, and in particular to a kind of SiC flexible ceramics constructed by nano wire
And preparation method thereof.
Background technology
Ceramic material has many excellent performances, such as high temperature resistant, corrosion-resistant, ageing-resistant, but generally fragility is larger,
Deflection is 0.1%~0.2% or even more hour will occur brittle fracture, therefore its mechanical resistant/thermal shock resistance properties is poor,
Application is limited by very large.
In recent years, researcher prepares the elastomer material material for being assembled and being formed by carbon nanocoils/pipe successively.2010
Year, X.C.Gui et al. uses CVD method, and the carbon nano tube three-dimensional network structural wood of flexible restorability is prepared first
Material, the material is entwined by CNT, and density is only 5~10mg/cm3.Under compression stress effect, when strain is 60%
Within when, the complete resilience of material, is not almost plastically deformed after unloading；Under the conditions of pulsating stress, material by 10 times circulate after,
Only about 10% or so residual is plastically deformed.2012, H.W.Liang et al. was prepared using ultra-fine Te nano wires as template
A kind of porous carbon nanofiber aeroge with the elasticity of compression gone out.2013, Z.Y.Wu et al. was using bacteria cellulose as mould
Plate, prepare it is ultralight, can elastic recovery carbon nanocoils aeroge, density of material is 4-6mg/cm3, maximum can recovery strain amount
For 90%.2014, S.Yang et al. prepared hyperelastic nanofiber aeroge using freeze-drying, and density is only
0.12mg/cm3, maximum can recovery strain amount be 80%, simultaneously as the high porosity, its room temperature thermal conductivity is only
0.026W/(m·K)。
But carbon is easily aoxidized in high temperature aerobic environment, the porous material that above-mentioned carbon nanocoils (pipe) are constituted is in high temperature etc.
It is difficult with adverse circumstances.SiC is a kind of high-modulus, dystectic advanced ceramics, with excellent high temperature resistant, it is anti-oxidant,
The advantages of anticorrosive, anti-thermal shock, while also having the fragility of ceramic material.One dimension SiC Nano fiber not only has above-mentioned SiC ceramic
Advantage, also with the good elastoplasticity different from block SiC ceramic.J.Wang etc. by molecular dynamics simulation,
Y.F.Zhang, X.D.Han, Z.J.Lin, G.M.Cheng et al. have found that SiC receives by in-situ scanning or transmission electron microscope observing
Rice noodles have certain elastoplasticity.In addition, SiC nanowire can be stabilized in 1000 DEG C, vacuum or inert atmosphere in atmosphere
1600 DEG C can be stabilized to, extraordinary high-temperature stability is shown.Therefore, the flexible ceramic constructed by SiC nanostructureds, will
Overcome the not oxidation resistant shortcoming of porous material of carbon nanocoils/pipe composition, realize that material has good elastoplasticity, ultralow heat conduction system
Number, extremely-low density, and good high-temperature oxidation resistance.Presently relevant research has no report.
The content of the invention
It is an object of the invention to provide a kind of SiC flexible ceramics constructed by nano wire and preparation method thereof, this method
Simple to operate, short preparation period is adapted to amplification production；Through SiC flexible ceramics intensity is good, elastoplasticity is high made from this method, every
Hot property is excellent.
The present invention is to be achieved through the following technical solutions：
A kind of preparation method of SiC flexible ceramics constructed by nano wire disclosed by the invention, comprises the following steps：
1) using alkoxy silane, distilled water as raw material, using ethanol as solvent, acid prepares poly- silicon as catalyst, hydrolysis
Oxygen alkane colloidal sol；
2) using porous carbon materials or porous carbon fiber material as skeleton, polysiloxanes is immersed to inside it by negative pressure impregnation
Colloidal sol；
3) by step 2) dipping after sample stand, formed ceramic forerunner, ceramic forerunner is then put into vacuum and done
Persistently handled in dry case to the complete gelation of colloidal sol, 1400~1600 DEG C are then heated in argon gas and is cracked, insulation 0.5~
2h, cools to room temperature with the furnace；
4) sample after cracking is placed in air furnace, 1~3h is incubated at 800~1000 DEG C, be made by nano wire structure
The SiC flexible ceramics built.
Step 1) alkoxy silane include dimethyldimethoxysil,ne and MTMS, dimethyl two
The mass ratio of methoxy silane and MTMS is (2~6):1.
Wherein, distilled water is added according to alkyl oxosilane complete hydrolysis aequum.
Step 1) acid uses concentration for 1mol/L nitric acid or hydrochloric acid.
Step 1) hydrolysis is 2~6h of processing at 40~90 DEG C, control polysiloxanes colloidal sol for 6~15mPas.
The porosity of porous carbon materials or the porous carbon fiber material is 75%~90%.
Step 2) negative pressure impregnation is that under 82~103kPa and room temperature condition, the polysiloxanes colloidal sol prepared is fallen
Suction is immersed in the skeleton of porous carbon materials or porous carbon fiber material, keeps 2h.
Step 3) in, ceramic forerunner is put into vacuum drying chamber, 8~12h is handled in 70~90 DEG C.
Step 4) in, the sample after cracking is placed in air furnace, from room temperature, with 5 DEG C/min heating rate, heating
To 800~1000 DEG C.
The invention also discloses using the SiC flexible ceramics constructed made from above-mentioned preparation method by nano wire.
Compared with prior art, the present invention has following beneficial technique effect：
The preparation method of the SiC flexible ceramics disclosed by the invention constructed by nano wire, is with porous carbon materials or porous
Carbon fibre material is skeleton, hydrolyzes the polysiloxanes colloidal sol prepared as presoma using alkoxy silane, passes through dipping-cracking-gas
Phase reaction, obtains porous carbon materials or porous carbon fiber material/SiC nanowire intermediate structure, is then removed by thermal oxide many
Hole carbon fiber skeleton, obtains the SiC flexible ceramics constructed by nano wire.This method is cracked and chemical gas phase reaction using presoma
The design being combined, in-situ preparation and self assembly by SiC nanowire prepare the SiC flexible ceramics that nano wire is constructed.This hair
Bright method can realize large scale, the preparation of complex-shaped SiC flexible ceramics, while short preparation period, cost is low, suitable for work
Industry metaplasia is produced.
Further, in course of reaction, by adjusting raw material and proportioning, can control polysiloxanes precursor colloidal sol into
Divide and structure.
Further, by adjusting the method that centrifugal drying removes unnecessary colloidal sol after dissolved adhesiveness, dipping time, and dipping,
Control the density of elastomer.
Through made from the inventive method by SiC nanowire by be self-assembly of have some strength, good elastoplasticity,
The lightweight three-dimensional net structure of excellent thermal insulation performance, can be used as high temperature insulating material, and in catalyst carrier, tissue work
In terms of journey, electrode material, damping energy-absorbing, impact resistance, with potential application value.
Brief description of the drawings
Fig. 1 is the SEM microscopic appearances of SiC flexible ceramics produced by the present invention；
Fig. 2 is the XRD spectra of SiC flexible ceramics produced by the present invention；
Fig. 3 is material compression stress-strain result of SiC flexible ceramics produced by the present invention；Wherein, (a) is not
Under the conditions of same compressive strain (20%, 40%, 60%, 80%), single compressive stress strain curve；(b) it is to set strain as 60%
When compression process (respectively correspond to left figure in 3 points of A, B, C)
The thermal conductivity of Fig. 4 SiC flexible ceramics produced by the present invention.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
It is that 10mm × 10mm × 10mm, density are 0.20g/cm that the present embodiment, which is prepared for a kind of size,3SiC elasticity pottery
Porcelain, is comprised the following steps that：
Step 1：With dimethyldimethoxysil,ne 20g, MTMS 10g, mixed with 12.3g distilled water,
Ethanol 10g is solvent, and the nitric acid that addition 2ml concentration is 1mol/L, 90 DEG C of hydrolysis 2h obtain the poly- silica that viscosity is 12mPas
Alkane colloidal sol.
Step 2：By 10mm × 10mm of size × 10mm porous carbon fiber material is skeleton, by negative pressure impregnation, to
The polysiloxanes colloidal sol that its internal immersion viscosity is 12mPas.
Step 3：Sample after dipping is positioned over 12h in surrounding environment, ceramic forerunner is formed, 70 DEG C of vacuum is put into
Continuing 8h in drying box makes the abundant gelation of colloidal sol in porous carbon fiber material.Then 1500 DEG C are heated in argon gas to split
Solution, is incubated 1h, cools to room temperature with the furnace.
Step 4：Sample after cracking is placed in air furnace, 2h is incubated at 900 DEG C, it is fine to remove porous carbon by thermal oxide
Material skeleton is tieed up, acquisition size is 10mm × 10mm × 10mm SiC flexible ceramics.
Embodiment 2
It is that 20mm × 20mm × 20mm, density are 0.17g/cm that the present embodiment, which is prepared for a kind of size,3SiC elasticity pottery
Porcelain, is comprised the following steps that：
Step 1：With dimethyldimethoxysil,ne 40g, MTMS 10g, mixed with 18.6g distilled water,
Ethanol 20g is solvent, and the nitric acid that addition 4ml concentration is 1mol/L hydrolyzes 6h at 50 DEG C, obtains the poly- silicon that viscosity is 15mPas
Oxygen alkane colloidal sol.
Step 2：By 20mm × 20mm of size × 20mm porous carbon fiber material is skeleton, by negative pressure impregnation, to
The polysiloxanes colloidal sol that its internal immersion viscosity is 15mPas.
Step 3：Sample after dipping is positioned over 12h in surrounding environment, ceramic forerunner is formed, 70 DEG C of vacuum is put into
Continuing 12h in drying box makes the abundant gelation of colloidal sol in porous carbon fiber material.Then 1600 DEG C are heated in argon gas to split
Solution, is incubated 2h, cools to room temperature with the furnace.
Step 4：Sample after cracking is placed in air furnace, 3h is incubated at 1000 DEG C, porous carbon is removed by thermal oxide
Fibrous material skeleton, acquisition size is 20mm × 20mm × 20mm SiC flexible ceramics.
Embodiment 3
It is that 10mm × 10mm × 10mm, density are 0.13g/cm that the present embodiment, which is prepared for a kind of size,3SiC elasticity pottery
Porcelain, is comprised the following steps that：
Step 1：With dimethyldimethoxysil,ne 20g, MTMS 3g, mixed with 6.8g distilled water, second
Alcohol 15g is solvent, and the nitric acid that addition 2ml concentration is 1mol/L hydrolyzes 2h at 40 DEG C, obtains the poly- silica that viscosity is 6mPas
Alkane colloidal sol.
Step 2：By 10mm × 10mm of size × 10mm porous carbon fiber material is skeleton, by negative pressure impregnation, to
The polysiloxanes colloidal sol that its internal immersion viscosity is 6mPas.After colloidal sol is fully absorbed, being put into centrifuge, (rotating speed is
1500r/min, centrifugation time is 30s), get rid of unnecessary colloidal sol.
Step 3：The sample impregnated after centrifugation is positioned over 12h in surrounding environment, ceramic forerunner is formed, is put into 70 DEG C
Continuing 12h in vacuum drying chamber makes the abundant gelation of colloidal sol in porous carbon fiber material.1400 are then heated in argon gas
DEG C cracking, be incubated 1h, cool to room temperature with the furnace.
Step 4：Sample after cracking is placed in air furnace, 1h is incubated at 800 DEG C, it is fine to remove porous carbon by thermal oxide
Material skeleton is tieed up, acquisition size is 10mm × 10mm × 10mm SiC flexible ceramics.
Porous carbon fiber material used in embodiment 1~3 is hard carbon fiber felt, and density is~0.22g/cm3, stomata
Rate is 82%, is produced by Lanzhou carbon fiber bar factory.
It is produced by the present invention that the three-dimensional net structure that overlap joint is formed mutually is wound by SiC nanowire, referring to Fig. 1 and Fig. 2.It is right
Material apply single shaft single compression stress when, referring to Fig. 3, wherein, (a) be different compressive strain (20%, 40%, 60%,
80%) under the conditions of, single compressive stress strain curve；(b) it is that the compression process set when strain is 60% (corresponds to a left side respectively
3 points of A, B, C in figure), it can be seen that：(1) even if material setting strain reaches 80%, also not by conquassation, remained in that complete
Whole property；(2) with the increase of deformation quantity, the amount of plastic deformation increase that material is produced after deformation, maximum plastic deformation amount after unloading
Up to about 68%.This explanation SiC flexible ceramic has certain elastoplasticity really, overcomes ceramic block material fragility easy
The characteristics of fracture.Using laser heat conduction method, test material thermal conductivity factor under argon gas, its room temperature thermal conductivity is only 0.015W/
(mK) excellent heat-proof quality, is shown, referring to Fig. 4.
Embodiment 4
It is that 10mm × 10mm × 10mm, density are 0.05g/cm that the present embodiment, which is prepared for a kind of size,3SiC elasticity pottery
Porcelain, is comprised the following steps that：
Step 1：With dimethyldimethoxysil,ne 20g, MTMS 5g, mixed with 6.8g distilled water, second
Alcohol 15g is solvent, and the nitric acid that addition 2ml concentration is 1mol/L hydrolyzes 2h at 40 DEG C, obtains the poly- silica that viscosity is 6mPas
Alkane colloidal sol.
Step 2：By 10mm × 10mm of size × 10mm cracking carbon connection carbon fibre material (CBCF) is skeleton, pass through
Negative pressure impregnation, to it inside immersion viscosity be 6mPas polysiloxanes colloidal sol.After colloidal sol is fully absorbed, centrifuge is put into
(rotating speed is 1500r/min, and centrifugation time is 200s), gets rid of unnecessary colloidal sol.
Step 3：The sample impregnated after centrifugation is positioned over 12h in surrounding environment, ceramic forerunner is formed, is put into 70 DEG C
Continuing 12h in vacuum drying chamber makes the abundant gelation of the colloidal sol in CBCF.1400 DEG C of cracking, insulation are then heated in argon gas
1h, cools to room temperature with the furnace.
Step 4：Sample after cracking is placed in air furnace, 1h is incubated at 800 DEG C, CBCF bones are removed by thermal oxide
Frame, acquisition size is 10mm × 10mm × 10mm SiC flexible ceramics.
Cracking carbon connection carbon fibre composite (Carbon-bonded carbon fiber used in the present embodiment
Composites, CBCF) provided as Aerospace Material ＆ Technology Inst. belonging to China Academy of Launch Vehicle Technology, numbering is
1-VIII。
Embodiment 5
It is that 10mm × 10mm × 10mm, density are 0.05g/cm that the present embodiment, which is prepared for a kind of size,3SiC elasticity pottery
Porcelain, is comprised the following steps that：
Step 1：With dimethyldimethoxysil,ne 20g, MTMS 5g, mixed with 6.8g distilled water, second
Alcohol 15g is solvent, and the nitric acid that addition 2ml concentration is 1mol/L hydrolyzes 2h at 40 DEG C, obtains the poly- silica that viscosity is 6mPas
Alkane colloidal sol.
Step 2：By 10mm × 10mm of size × 10mm porous carbon materials are skeleton, by negative pressure impregnation, to it in
The polysiloxanes colloidal sol that portion's immersion viscosity is 6mPas.After colloidal sol is fully absorbed, being put into centrifuge, (rotating speed is 1500r/
Min, centrifugation time is 200s), get rid of unnecessary colloidal sol.
Step 3：The sample impregnated after centrifugation is positioned over 12h in surrounding environment, ceramic forerunner is formed, is put into 70 DEG C
Continuing 12h in vacuum drying chamber makes the abundant gelation of the colloidal sol in porous carbon materials.Then 1400 DEG C are heated in argon gas to split
Solution, is incubated 1h, cools to room temperature with the furnace.
Step 4：Sample after cracking is placed in air furnace, 1h is incubated at 800 DEG C, porous carbon is removed by thermal oxide
Expect skeleton, acquisition size is 10mm × 10mm × 10mm SiC flexible ceramics.
Porous carbon materials used in embodiment 5 are to be obtained by polyurethane foam under Ar through 800 DEG C of charing 2h, used poly-
The hole size of urethane foam is 0.8~1.2mm, and size of struts is 0.1~0.25mm, is purchased from the limited public affairs of enlightening filtering material in Luoyang
Department.
Claims (9)
1. a kind of preparation method for the SiC flexible ceramics constructed by nano wire, it is characterised in that comprise the following steps：
1) using alkoxy silane, distilled water as raw material, using ethanol as solvent, acid is as catalyst, and hydrolysis prepares polysiloxanes
Colloidal sol；
2) it is molten to immersion polysiloxanes inside it by negative pressure impregnation using porous carbon materials or porous carbon fiber material as skeleton
Glue；
3) by step 2) dipping after sample stand, formed ceramic forerunner, ceramic forerunner is then put into vacuum drying chamber
In persistently handle to the complete gelation of colloidal sol, be then heated in argon gas 1400~1600 DEG C cracking, be incubated 0.5~2h, with
Stove is cooled to room temperature；
4) sample after cracking is placed in air furnace, 1~3h is incubated at 800~1000 DEG C, be made what is constructed by nano wire
SiC flexible ceramics.
2. the preparation method of the SiC flexible ceramics according to claim 1 constructed by nano wire, it is characterised in that step
1) alkoxy silane include dimethyldimethoxysil,ne and MTMS, dimethyldimethoxysil,ne and
The mass ratio of MTMS is (2~6):1.
3. the preparation method of the SiC flexible ceramics according to claim 1 constructed by nano wire, it is characterised in that step
1) acid uses concentration for 1mol/L nitric acid or hydrochloric acid.
4. the preparation method of the SiC flexible ceramics according to claim 1 constructed by nano wire, it is characterised in that step
1) hydrolysis is 2~6h of processing at 40~90 DEG C, and it is 6~15mPas to control polysiloxanes colloidal sol.
5. the preparation method of the SiC flexible ceramics according to claim 1 constructed by nano wire, it is characterised in that described
The porosity of porous carbon materials or porous carbon fiber material is 75%~90%.
6. the preparation method of the SiC flexible ceramics according to claim 1 constructed by nano wire, it is characterised in that step
2) negative pressure impregnation is under 82~103kPa and room temperature condition, the polysiloxanes colloidal sol suck-back prepared to be immersed in porous
In the skeleton of carbon material or porous carbon fiber material, 2h is kept.
7. the preparation method of the SiC flexible ceramics according to claim 1 constructed by nano wire, it is characterised in that step
3) in, ceramic forerunner is put into vacuum drying chamber, 8~12h is handled in 70~90 DEG C.
8. the preparation method of the SiC flexible ceramics according to claim 1 constructed by nano wire, it is characterised in that step
4) in, the sample after cracking is placed in air furnace, from room temperature, with 5 DEG C/min heating rate, 800~1000 are warming up to
℃。
9. the SiC flexible ceramics constructed by nano wire are made using the preparation method described in any one in claim 1~8.
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