CN105801122B - A kind of preparation method of graded pore structure silicon carbide-based porous ceramics - Google Patents
A kind of preparation method of graded pore structure silicon carbide-based porous ceramics Download PDFInfo
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Abstract
The invention belongs to the preparation fields of porous ceramic film material, and in particular to a kind of preparation method of graded pore structure silicon carbide-based porous ceramics.The preparation method of a kind of graded pore structure silicon carbide-based porous ceramics proposed=use carborundum porous ceramics as matrix, the nano-grade silicon nitride whisker that one layer of aperture is less than carborundum porous ceramics aperture is coated on the surface of carborundum porous ceramics, the graded pore structure silicon carbide-based porous ceramics that aperture from inside to outside becomes larger are formed, include the coating and atmosphere sintering Four processes of the pretreatment of carborundum porous ceramics, the preparation of silicon slurry, silicon slurry on carborundum porous ceramics surface.The present invention is by coating the nano-grade silicon nitride whisker that one layer of aperture is less than carborundum porous ceramics aperture on the surface of carborundum porous ceramics, the graded pore structure silicon carbide-based porous ceramics that aperture from inside to outside becomes larger are formed, its durability is improved under the premise of not reducing filter element service performance.
Description
Technical field
The invention belongs to the preparation technical fields of porous ceramic film material, and in particular to a kind of graded pore structure is silicon carbide-based more
The preparation method of hole ceramics.
Background technique
With China's industrial boom, environmental pressure is increasing；Whenever winter approached, haze and PM2.5 can be at
For hot spot concerned by people；The fast sale of various air purifiers can only also play a role in the confined space indoors；It wants
Think fundamentally to alleviate and improve atmosphere polluting problem, need to be limited and be administered from industrial discharge side；Electric precipitation is to fine
The removal rate of particle is high, but the operating cost as brought by power consumption is very high, is limited operation stability lower than 350 °C by method；
Cyclone dust removal is used since operating cost is lower by many enterprises；But cyclone dust removal is for subparticle especially partial size
In 5 particles below, removal efficiency is lower；Meanwhile lower running temperature also results in a large amount of latent heat waste；Porous ceramics
Filter is due to running temperature height, operating cost more low advantage high to the removal rate of subparticle, by more industry enterprises
Industry is of interest and uses.
For currently used filter element in order to guarantee higher filtering rate, porous ceramic matrices suitable is usually with higher
The porosity and biggish air vent aperture；Meanwhile in order to improve filtering accuracy, one can be covered in the outer side surface of porous ceramic matrices suitable
Layer has the membrane structure of more small-bore；During military service, due to prolonged thermal shock, burn into blowback, film knot usually will cause
It the destruction of structure and falls off.
Summary of the invention
The purpose of the present invention is to propose to a kind of preparation methods of graded pore structure silicon carbide-based porous ceramics, by being carbonized
The surface of silicon porous ceramics coats the nano-grade silicon nitride whisker that one layer of aperture is less than carborundum porous ceramics aperture, is formed by interior
The graded pore structure silicon carbide-based porous ceramics that outside aperture becomes larger, under the premise of not reducing filter element service performance
Improve its durability.
The present invention is to complete foregoing invention purpose to adopt the following technical scheme that
A kind of preparation method of graded pore structure silicon carbide-based porous ceramics, the preparation method use silicon carbide porous
Ceramics are used as matrix, coat the nanoscale that one layer of aperture is less than carborundum porous ceramics aperture on the surface of carborundum porous ceramics
Silicon nitride crystal whisker forms the graded pore structure silicon carbide-based porous ceramics that aperture from inside to outside becomes larger, includes silicon carbide
The pretreatment of porous ceramics, the preparation of silicon slurry, silicon starch coating and atmosphere sintering Four processes on carborundum porous ceramics surface,
Its specific process step are as follows:
1) pretreatment of carborundum porous ceramics: carborundum porous ceramics are placed in deionized water, ultrasonic cleaning
20min, taking-up are placed in baking oven spare for 24 hours in 100 °C of drying；The porosity of the carborundum porous ceramics is 30~50%,
Average pore size is 80~200 μm；
2) preparation of silicon slurry: silicon powder, dispersing agent and deionized water are placed in a beaker, mechanical stirring makes it be uniformly dispersed
It is starched to water base silicon；The silicon powder average grain diameter is at 1~20 μm；The dispersing agent is tetramethylammonium hydroxide or polyethylene
One of imines；The silicon powder, dispersing agent are respectively 5~15%, the 0.3~1.5% of deionized water quality；
3) water base silicon slurry coating of the silicon slurry on carborundum porous ceramics surface: is coated in the table of carborundum porous ceramics
Face is stored at room temperature, and is subsequently placed in drying in baking oven and is obtained silicon carbide-based porous ceramics；
4) atmosphere sintering: the silicon carbide-based porous ceramics after drying being placed in atmosphere sintering furnace and are sintered, final
To the silicon carbide-based porous ceramics with graded pore structure.
Sintering process of the silicon carbide-based porous ceramics in atmosphere sintering furnace is, with the heating speed of 2-5 °C/min
Rate rises to 900 °C, rises to 1300-1400 °C with the heating rate of 0.2-1 °C/min, keeps the temperature Temperature fall after 1-3h.
The silicon slurry coating can choose the mode of spraying or brushing；Porous ceramics after coating is being stored at room temperature for 24 hours,
It is subsequently placed in baking oven in 90 °C of drying for 24 hours.
Atmosphere used in the atmosphere sintering furnace is nitrogen.
The preparation method of a kind of graded pore structure silicon carbide-based porous ceramics proposed by the present invention, by silicon carbide porous
The surface of ceramics coats the nano-grade silicon nitride whisker that one layer of aperture is less than carborundum porous ceramics aperture, using silicon and nitrogen it
Between nitridation reaction form aperture becomes larger from inside to outside graded pore structure in the superficial layer of carborundum porous ceramics, due to
The hole very little that close web frame is formed can effectively intercept the fine particle in air；Meanwhile the thickness of close web frame
Degree is very thin, and thus bring pressure drop very little, will not cause to be substantially reduced to the air penetrability of porous ceramics entirety；Due to having simultaneously
There are filtering accuracy and filtering rate, which can be applied to the filtering neck of high-temperature smoke
Domain；Its durability is improved under the premise of not reducing filter element service performance.
Detailed description of the invention
Fig. 1 show the fracture apperance photo of sample prepared by embodiment 1.
Specific embodiment
The present invention is illustrated in conjunction with following examples and drawings:
Embodiment 1
Selecting the porosity is 30%, and the silicon carbide-based even porous ceramics that average pore size is 80 μm are placed in deionized water,
It is cleaned by ultrasonic 20min, after taking-up for 24 hours in 100 °C of drying.By average grain diameter in 1 μm of silicon powder 5g, dispersing agent TMAH 0.3g and
Deionized water 100g is placed in a beaker, and mechanical stirring obtains water base silicon slurry；Silicon is starched into spraying or is brushed silicon carbide-based uniformly more
The surface of hole ceramics, is stored at room temperature for 24 hours, then for 24 hours in 90 °C of drying；It transfers them in atmosphere sintering furnace and is sintered, lead to
Enter nitrogen atmosphere, rise to 900 °C with the heating rate of 2 °C/min, rises to 1300 °C with the heating rate of 1 °C/min, keep the temperature 3h
Temperature fall afterwards.Gained graded pore structure silicon carbide-based porous ceramics are as shown in Figure 1.
Embodiment 2
Selecting the porosity is 37%, and the silicon carbide-based even porous ceramics that average pore size is 160 μm are placed in deionized water,
It is cleaned by ultrasonic 20min, after taking-up for 24 hours in 100 °C of drying.Silicon powder 10g, dispersing agent PEI 0.6g by average grain diameter at 5 μm
It is placed in a beaker with deionized water 100g, mechanical stirring obtains water base silicon slurry；Silicon is starched into spraying or is brushed silicon carbide-based uniform
The surface of porous ceramics is stored at room temperature for 24 hours, then for 24 hours in 90 °C of drying.It transfers them in atmosphere sintering furnace and is sintered,
It is passed through nitrogen atmosphere, rises to 900 °C with the heating rate of 5 °C/min, 1350 °C is risen to the heating rate of 0.5 °C/min, protects
Temperature fall after warm 2h.
Embodiment 3
Selecting the porosity is 50%, and the silicon carbide-based even porous ceramics that average pore size is 200 μm are placed in deionized water,
It is cleaned by ultrasonic 20min, after taking-up for 24 hours in 100 °C of drying；Silicon powder 15g, dispersing agent TMAH 1.5g by average grain diameter at 20 μm
It is placed in a beaker with deionized water 100g, mechanical stirring obtains water base silicon slurry.Silicon is starched into spraying or is brushed silicon carbide-based uniform
The surface of porous ceramics is stored at room temperature for 24 hours, then for 24 hours in 90 °C of drying.It transfers them in atmosphere sintering furnace and is sintered,
It is passed through nitrogen atmosphere, rises to 900 °C with the heating rate of 3 °C/min, 1400 °C is risen to the heating rate of 0.2 °C/min, protects
Temperature fall after warm 1h.
Embodiment 4
Selecting the porosity is 37%, and the silicon carbide-based even porous ceramics that average pore size is 160 μm are placed in deionized water,
It is cleaned by ultrasonic 20min, after taking-up for 24 hours in 100 °C of drying.Silicon powder 10g, dispersing agent PEI 1.2g by average grain diameter at 10 μm
It is placed in a beaker with deionized water 100g, mechanical stirring obtains water base silicon slurry.Silicon is starched into spraying or is brushed silicon carbide-based uniform
The surface of porous ceramics is stored at room temperature for 24 hours, then for 24 hours in 90 °C of drying.It transfers them in atmosphere sintering furnace and is sintered,
It is passed through nitrogen atmosphere, rises to 900 °C with the heating rate of 3 °C/min, 1370 °C is risen to the heating rate of 0.5 °C/min, protects
Temperature fall after warm 2h.
Claims (2)
1. a kind of preparation method of graded pore structure silicon carbide-based porous ceramics, it is characterised in that: the preparation method uses
Carborundum porous ceramics coat one layer of partial size on the surface of carborundum porous ceramics and are less than carborundum porous ceramics hole as matrix
The silicon powder of diameter forms the gradually smaller graded pore structure silicon carbide-based porous ceramics in aperture from inside to outside, includes that silicon carbide is more
The pretreatment of hole ceramics, the preparation of silicon slurry, silicon starch coating and atmosphere sintering Four processes on carborundum porous ceramics surface,
Specific process step are as follows:
1) pretreatment of carborundum porous ceramics: carborundum porous ceramics are placed in deionized water, are cleaned by ultrasonic 20min, are taken
It is placed in baking oven out spare for 24 hours in 100 °C of drying；The porosity of the carborundum porous ceramics is 30~50%, average pore size
It is 80~200 μm；
2) preparation of silicon slurry: silicon powder, dispersing agent and deionized water are placed in a beaker, mechanical stirring makes it be uniformly dispersed to obtain water
Base silicon slurry；The silicon powder average grain diameter is at 1~20 μm；The dispersing agent is tetramethylammonium hydroxide or polyethyleneimine
One of；The silicon powder, dispersing agent are respectively 5~15%, the 0.3~1.5% of deionized water quality；
3) water base silicon slurry coating of the silicon slurry on carborundum porous ceramics surface: is coated in the surface of carborundum porous ceramics, room
Temperature is stood, and is subsequently placed in drying in baking oven and is obtained silicon carbide-based porous ceramics；
4) atmosphere sintering: the silicon carbide-based porous ceramics after drying are placed in atmosphere sintering furnace and are sintered, tool is finally obtained
There are the silicon carbide-based porous ceramics of graded pore structure；Atmosphere used in the atmosphere sintering furnace is nitrogen；The carbonization
Sintering process of the silicon substrate porous ceramics in atmosphere sintering furnace is 900 °C to be risen to the heating rate of 2-5 °C/min, with 0.2-
The heating rate of 1 °C/min rises to 1300-1400 °C, keeps the temperature Temperature fall after 1-3h.
2. a kind of preparation method of graded pore structure silicon carbide-based porous ceramics as described in claim 1, it is characterised in that: institute
The silicon slurry coating stated can choose the mode of spraying or brushing；Porous ceramics after coating is being stored at room temperature for 24 hours, is subsequently placed in baking
In case for 24 hours in 90 °C of drying.
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| CN106478107B (en) * | 2016-10-17 | 2019-05-10 | 武汉科技大学 | A kind of silicon nitride crystal whisker silicon carbide porous ceramics and preparation method thereof |
| CN112479734A (en) * | 2017-08-03 | 2021-03-12 | 福建省德化县华晨陶瓷有限公司 | Wear-resistant high-low temperature-resistant ceramic product |
| CN108794073A (en) * | 2018-05-29 | 2018-11-13 | 绍兴市鼎泰节能环保科技有限公司 | A kind of dedusting agent and preparation method thereof |
| CN112759418B (en) * | 2021-01-08 | 2022-05-13 | 武汉科技大学 | Silicon nitride whisker reinforced corundum porous ceramic filter and preparation method thereof |
| CN115414798B (en) * | 2022-08-19 | 2024-03-29 | 电子科技大学长三角研究院(湖州) | Preparation method and application of silicon nitride-based ceramic separation membrane with micro-nano composite fiber structure |
| CN115893979B (en) * | 2022-11-09 | 2024-03-01 | 新明珠集团股份有限公司 | Preparation method of fragrance slow-release ceramic with multi-stage pore size structure |
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