CN108218467A - A kind of preparation method of high porosity and lower thermal conductivity porous nano silicon carbide ceramics - Google Patents
A kind of preparation method of high porosity and lower thermal conductivity porous nano silicon carbide ceramics Download PDFInfo
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Abstract
The present invention relates to porous ceramic film material field, the method for specially a kind of porous nano thyrite that high porosity and lower thermal conductivity are prepared by pore creating material method.This method is using β SiC nano particles and micron flakes graphite as raw material, using ethyl alcohol as medium, carries out ball milling mixing, forms slurry；Sieve is pressed into green body with mold, is then further densified under cold isostatic pressure into powder after slurry drying；Green body is subjected to high temperature pressure-free sintering in argon gas atmosphere, then heat treatment removal pore creating material graphite, acquisition have both the porous nano thyrite of micron openings and nano-pore in air.The present invention can prepare high porosity (54~76%) and lower thermal conductivity (0.74~0.14W m with hierarchical porous structure and controlled porosity‑1K‑1) porous nano SiC ceramic material.
Description
Technical field
The present invention relates to porous ceramic film material fields, and specially one kind prepares high porosity by pore creating material method and low-heat is led
The method of the porous nano thyrite of rate.
Background technology
The cutting edge technology application of heat-insulated and energy conversion etc. is required for lower thermal conductivity and high reliability under high temperature
New material.Nano structural material becomes academic and technical field research hotspot due to its good heat-proof quality.They
The fundamental mechanism of thermal resistance is originated from interface resistance huge in nanostructured.However, with the reduction of particle size, the ratio table of material
Area increases, and the high high-temp stability of nanostructured is caused drastically to decline.Oxide-based nanomaterial to be applied is led at present, such as：
Silica (SiO2) and aluminium oxide (Al2O3) aeroge and its composite material, thermostabilization be below 1200 DEG C.Therefore, at present
The bottleneck problem for being badly in need of solving is how in novel nano-material while to realize extremely low thermal conductivity and high thermal stability.
Silicon carbide ceramics can show excellent mechanical property and corrosion resistance in harsh hot environment, thus in work
Industry field has a wide range of applications.Importantly, due to strong Si-C covalent bonds and low self-diffusion coefficient, it was reported that cold pressing
The SiC powder block of preparation can maintain the initial sample dimension of its room temperature in 1800 DEG C of high temperature, not occur acutely to shrink
(M.Fukushima et al.Mater.Sci.Eng.B 2008(148):211–214.).And β-SiC have the phase of superelevation
Stability does not have phase transition (B.K.Jang et al.Adv.Mater.2007 (8) within 2000 DEG C:655–659.).Although
SiC is a kind of Thermal Conductivity Ceramics Used, but when particle size is reduced to Nano grade, nano SiC show it is amazing every
Hot property (P.Wan et al.Scripta Mater.2017 (128):1-5).Therefore, porous nano silicon carbide ceramics is a kind of
Great potential, applied to the high temperature heat-resistant insulation in Aeronautics and Astronautics field and thermally protective materials.
Invention content
The purpose of the present invention is to provide the preparations of a kind of high porosity and the porous nano silicon carbide ceramics of lower thermal conductivity
Method makes SiC porous ceramics have completely new lower thermal conductivity performance characteristics.
Technical scheme is as follows：
The preparation method of a kind of high porosity and lower thermal conductivity porous nano silicon carbide ceramics, carbofrax material are received to be porous
Rice SiC ceramic, is as follows：
1) preparation of slurry：Using β-SiC nano particles and graphite powder mass ratio as 9:1~5:5 preparation raw materials, using ethyl alcohol as
Medium, carries out ball milling mixing 8~16 hours, forms slurry；
2) sieve into powder, is pressed into green body, then 10 under the cold isostatic pressure of 200~240MPa with mold after slurry drying
Further densification in~30 minutes；
3) green body is carried out to high temperature pressure-free sintering 1~3 hour in 1400~1600 DEG C of argon gas atmospheres, then in air
600~800 DEG C of heat treatment, 3~5 hours removal pore creating material graphite, obtains the porous nano silicon carbide for having both micron openings and nano-pore
Ceramic material.
The high porosity and the preparation method of lower thermal conductivity porous nano silicon carbide ceramics, porous nano SiC ceramic
The porosity ranges of material are 54~76%, and micron openings is uniformly distributed in thin slice and shape, and pore size is length and width：2 μm~6.5 μm,
It is thick：0.5~1.5 μm；Nano-pore is distributed on the skeleton of the ceramic material, pore diameter range ＜ 50nm.
The high porosity and the preparation method of lower thermal conductivity porous nano silicon carbide ceramics, β-SiC nano particles
Average grain size is 20~50nm, and the particle diameter distribution of graphite powder is D90=6.5 μm.
The high porosity and the preparation method of lower thermal conductivity porous nano silicon carbide ceramics, the heating speed of high temperature sintering
Rate：Less than 1000 DEG C are 8~12 DEG C/min, and 1000 DEG C or more are 4~6 DEG C/min.
Advantages of the present invention and advantageous effect are：
1. the present invention proposes to prepare the porous nano silicon carbide ceramics material of high porosity and lower thermal conductivity by pore creating material method
The method of material, this method can prepare the high porosity for having both micron openings and nano-pore and controlled porosity and lower thermal conductivity
SiC porous ceramics.
2. the present invention's is easy to operate, it need to only pass through the streams such as preparation, compression moulding, high temperature sintering and the carbon removal treatment of slurry
Journey.
3. the present invention is easy to mass produce without special installation.
4. the present invention can be prepared with higher porosity porous nano SiC ceramic material, the porous ceramics is with multilayer
Secondary nanostructured thermal resistance mechanism and hierarchical porous structure can greatly reduce thermal conductivity, be that the lightening fire resistant of function admirable is exhausted
Hot material.
In short, this method using β-SiC nano particles and micron flakes graphite as raw material, after 12 hours ball millings, obtains
Uniformly mixed powder.Powder after 220MPa cold isostatic compactions, carried out in 1500 DEG C of argon gas atmospheres 2 hours without pressure burn
Knot, 700 DEG C of heat treatments remove graphite pore former in 4 hours to subsequent sample in air, finally prepare porous nano SiC ceramic.
The simple for process of the method for the present invention, operability are strong, can prepare the high hole with Hierarchical porosity structure and controlled porosity
Gap rate (54~76%) and lower thermal conductivity (0.74~0.14W m-1K-1) porous nano SiC ceramic material.
Description of the drawings
Fig. 1 is the transmission electron microscope photo of SiC nano-powder in embodiment 1.In figure, the illustration on top is under high-amplification-factor
Single SiC nano particles shape appearance figure；The illustration of lower part is SiC nano-powder entirety shape appearance figure under low amplification factor.
Fig. 2 (a) is porous nano the three-dimensional imaging of SiC ceramic material X-ray diffraction (XRT) figure in embodiment 2.
Fig. 2 (b) is scanning electron microscope (SEM) photo of porous nano SiC ceramic material in embodiment 2.
Specific embodiment
In specific implementation process, porous nano silicon carbide (SiC) ceramics of high porosity and lower thermal conductivity of the present invention
Preparation method is as follows：
1) preparation of slurry：It is respectively with β-SiC nano particles and graphite powder mass ratio：9:1、8:2、7:3、6:4 and 5:5
Preparation raw material using ethyl alcohol as medium, carries out ball milling mixing 12 hours, forms slurry；Wherein, the average grain of β-SiC starting powders
Degree size is 35nm, and the particle diameter distribution of graphite powder is D90=6.5 μm.
2) sieve into powder, is pressed into green body, then in the isostatic cool pressing of 220MPa with the mold of required shape after slurry drying
It is further densified under power；
3) green body is subjected to high temperature pressure-free sintering in 1500 DEG C of argon gas atmospheres, then 700 DEG C of heat treatments are gone in air
Except pore creating material graphite, the SiC porous ceramic film materials for having both micron openings and nano-pore can be obtained.Porous nano SiC ceramic material
Porosity ranges for 54~76%, micron openings is uniformly distributed in thin slice and shape, and pore size is length and width：It is 2 μm~6.5 μm, thick：~
0.7 μm, be nano-pore on skeleton, pore diameter range ＜ 50nm.
The present invention is described in detail below by embodiment.
Embodiment 1
After a small amount of SiC nano-powder is put into ethyl alcohol ultrasonic disperse 30 minutes, with capillary glass tube drawing powder and second
Then the mixed liquor of alcohol drips 2~3 micro-grids for dripping to 200 mesh and supports on film that fully drying is observed after under transmission electron microscope, is such as schemed
1.The result shows that, contain a large amount of faults in β-SiC nano particles average grain diameter about 35nm and particle in the present embodiment.Tiny
Particle size generates big interface and crystal boundary thermal resistance, and lattice defect (such as fault) generates further resistance to the transmission for the phonon that conducts heat
Hinder, therefore can effectively reduce thermal conductivity.
Embodiment 2
It is 7 by β-SiC nano particles and graphite powder mass ratio:3 preparation raw materials, using ethyl alcohol as medium, in silicon nitride ball milling
Ball milling mixing is carried out in tank 12 hours, form slurry；Then sieve is pressed into powder with the mold of required shape after slurry is dried
Green body, then at the further densification in lower 10 minutes of the cold isostatic pressure of 220MPa；
Green body is carried out high temperature pressure-free in 1500 DEG C of argon gas atmospheres to be sintered 2 hours, then 700 DEG C of heat treatment in air
4 hours removal pore creating material graphite, obtains porous nano SiC ceramic material.In the present embodiment, the porosity of sample is 66.8%,
Thermal conductivity is 0.42W m-1K-1.The microscopic appearance of porous ceramics is shown that micron openings is in thin slice and shape by the XRT photos of Fig. 2 (a)
It is uniformly distributed, pore size is length and width：It is 2 μm~6.5 μm, thick：~0.7 μm.Nano-pore on porous ceramic skeleton is by Fig. 2's (b)
SEM photograph shows that intergranular there are nano-pore, pore diameter range ＜ 50nm.
Embodiment the result shows that, the present invention is combined using nanometer powder and pore creating material method simple for process, can pass through tune
The additive amount of pore creating material is saved to control porosity, there is higher porosity using porous nano SiC ceramic prepared by this method
And lower thermal conductivity, and the porous ceramics for having both micron openings and nano-pore can be prepared.
Claims (4)
- A kind of 1. preparation method of high porosity and lower thermal conductivity porous nano silicon carbide ceramics, which is characterized in that silicon carbide material Expect for porous nano SiC ceramic, to be as follows：1) preparation of slurry：Using β-SiC nano particles and graphite powder mass ratio as 9:1~5:5 preparation raw materials, using ethyl alcohol as Jie Matter, carries out ball milling mixing 8~16 hours, forms slurry；2) sieve into powder, is pressed into green body, then 10~30 under the cold isostatic pressure of 200~240MPa with mold after slurry drying Minute further densification；3) green body in 1400~1600 DEG C of argon gas atmospheres is carried out to high temperature pressure-free and is sintered 1~3 hour, then in air 600 3~5 hours removal pore creating material graphite of~800 DEG C of heat treatment, obtains the porous nano silicon carbide pottery for having both micron openings and nano-pore Ceramic material.
- 2. the preparation method of high porosity described in accordance with the claim 1 and lower thermal conductivity porous nano silicon carbide ceramics, special Sign is that the porosity ranges of porous nano SiC ceramic material are 54~76%, and micron openings is uniformly distributed in thin slice and shape, hole Size is length and width：It is 2 μm~6.5 μm, thick：0.5~1.5 μm；Nano-pore is distributed on the skeleton of the ceramic material, pore diameter range ＜ 50nm.
- 3. the preparation method of high porosity described in accordance with the claim 1 and lower thermal conductivity porous nano silicon carbide ceramics, special Sign is that the average grain size of β-SiC nano particles is 20~50nm, and the particle diameter distribution of graphite powder is D90=6.5 μm.
- 4. the preparation method of high porosity described in accordance with the claim 1 and lower thermal conductivity porous nano silicon carbide ceramics, special Sign is, the heating rate of high temperature sintering：Less than 1000 DEG C are 8~12 DEG C/min, and 1000 DEG C or more are 4~6 DEG C/min.
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Cited By (5)
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| CN109796196A (en) * | 2019-04-01 | 2019-05-24 | 西北工业大学 | A kind of preparation method of the superhigh temperature porous ceramic skeleton of morphology controllable |
| CN111947345A (en) * | 2020-07-17 | 2020-11-17 | 浙江吉成新材股份有限公司 | Water refrigeration method and water refrigeration device using porous material |
| CN111960846A (en) * | 2020-07-17 | 2020-11-20 | 浙江吉成新材股份有限公司 | Nano porous material and preparation method thereof |
| CN113045332A (en) * | 2021-02-08 | 2021-06-29 | 中国科学院金属研究所 | Ultrahigh-porosity high-entropy carbide ultrahigh-temperature ceramic and preparation method thereof |
| CN113897170A (en) * | 2021-10-27 | 2022-01-07 | 浙江先导热电科技股份有限公司 | Low-thermal-conductivity composite glue and application |
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