CN108264354A - Multichannel silicon carbide ceramic support body and preparation method thereof - Google Patents
Multichannel silicon carbide ceramic support body and preparation method thereof Download PDFInfo
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- CN108264354A CN108264354A CN201810075202.0A CN201810075202A CN108264354A CN 108264354 A CN108264354 A CN 108264354A CN 201810075202 A CN201810075202 A CN 201810075202A CN 108264354 A CN108264354 A CN 108264354A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/963—Surface properties, e.g. surface roughness
Abstract
The present invention provides a kind of multichannel silicon carbide ceramic support body and preparation method thereof, and the preparation method of wherein multichannel silicon carbide ceramic support body includes the following steps：S1, according to mass ratio 100:(5~10)：(3~5):(10~15) weigh carborundum powder I, carborundum powder II, bonding agent and pore creating material, wherein, the average grain diameter of the carborundum powder I is more than the average grain diameter of the carborundum powder II；The bonding agent is dissolved in water by S2, carborundum powder I, carborundum powder II and the pore creating material is added in the aqueous solution of the bonding agent, is mixed to get mixed material；S3 is kneaded the mixed material, obtains pug；The pug is carried out extrusion molding, obtains biscuit by S4；S5 is burnt into after the biscuit is dried, obtains multichannel silicon carbide ceramic support body.Silicon carbide ceramic support body according to the present invention has the advantages that intensity is high, flux is big.
Description
Technical field
The present invention relates to the preparing technical fields of ceramic material, and in particular, to a kind of multichannel silicon carbide ceramic membrane branch
Support body and preparation method thereof.
Background technology
More and more industrial wastewaters in recent years, especially heavy metal wastewater thereby just discharge wantonly without strictly handling, and cause
How the heavy metal pollution in waters, soil and environment, reduce heavy metal and have become an important topic to the pollution of environment.
Heavy metal wastewater thereby is typically derived from mining, metal smelt and processing, plating, process hides, pesticide, papermaking, paint, printing and dyeing, core
The industries such as technology and petrochemical industry, contained heavy metal ion are difficult to biodegradable and are easily enriched with by bio-absorbable, and toxicity has
Duration is the pollutant of a kind of great potential hazard.At present, it is big can be substantially divided into three for the method for heavy metal containing wastewater treatment
Class：(1) method that method of chemical treatment, i.e. heavy metal ions in wastewater are removed by the way that chemical reaction occurs；(2) physical treatment process,
The method that the heavy metal ion in waste water is made to be adsorbed, concentrated under conditions of its chemical form is not changed, detached；(3) it is raw
Object facture removes the side of heavy metal ions in wastewater by the effects that flocculation of microorganism or plant, uptake and accumulation, enrichment
Method.But all there is treatment process is longer, cost is higher, waste residue is more, introduces two to some extent in practice for these methods
Secondary pollution, the problems such as treatment conditions are harsh, treating capacity is limited.
The environment protectment protection being gradually increased in face of China, researcher are increasingly biased to utilize membrane separation technique processing weight
Metallic wastewater.In many seperation films, inorganic ceramic membrane is the important component of high performance membrane material, is by inorganic metal oxygen
The thin-film material for having the function of to efficiently separate that compound is prepared, it is good, anti-with high temperature resistant, resistance to chemical attack, mechanical strength
Microorganism ability is strong, permeation flux is big, clanability is strong, pore-size distribution is narrow, service life is long, is hardly damaged the advantages of waiting.Mesh
The research of preceding inorganic ceramic membrane is concentrated mainly on the membrane materials such as aluminium oxide, zirconium oxide, cordierite, and commercialized inorganic ceramic membrane is main
It is pellumina.However, the characteristics of heavy metal wastewater thereby is deep-etching, oil-containing, containing heavy metal ion.Ring is used in so harsh
Under border, the strong acid-base resistance corrosive power of alumina ceramic membrane is weak, therefore service life is low, the membrane material update cycle is short；Aluminium oxide is made pottery
The angle of wetting of porcelain film and pure water is about 30；Therefore filtration flux is small, waste water treatment efficiency is low.
Invention content
In view of this, the present invention provides a kind of preparation method of multichannel silicon carbide ceramic support body.
The present invention also proposes a kind of multichannel silicon carbide ceramic support body.
In order to solve the above technical problems, present invention employs following technical schemes：
The preparation method of the multichannel silicon carbide ceramic support body of embodiment according to a first aspect of the present invention, including as follows
Step：
S1, according to mass ratio 100:(5~10)：(3~5):(10~15) weigh carborundum powder I, carborundum powder II, combine
Agent and pore creating material, wherein, the average grain diameter of the carborundum powder I is more than the average grain diameter of the carborundum powder II；
The bonding agent is dissolved in water by S2, and carborundum powder I, carborundum powder II and the pore creating material are added in the knot
In the aqueous solution of mixture, mixed material is mixed to get, solid content is 50%~70%；
S3 is kneaded the mixed material, obtains pug；
The pug is carried out extrusion molding, obtains biscuit by S4；
S5 is burnt into after the biscuit is dried, obtains multichannel silicon carbide ceramic support body.
Preferably, between 35~55 μm, the carborundum powder II is averaged the average particle size range of the carborundum powder I
For particle size range between 0.5~3.0 μm, purity is more than 98%.
Preferably, in the step S1, the bonding agent is selected from sodium carboxymethylcellulose, sodium hydroxyethlcellulose, methyl
Cellulose, polyvinyl alcohol, polyacrylic acid and its mixture.
Preferably, the bonding agent is sodium carboxymethylcellulose, and viscosity is 10000~20000PaS, preferably
16000PaS, purity are more than 98.5%.
Preferably, in the step S1, the pore creating material be carbon black, activated carbon powder, corn flour or graphite powder, average grain diameter
Between 5~10 μm.
Further, in the step S3, the mixed material is put into vacuum deairing machine, extrusion pressure 0.08~
Under conditions of 0.12MPa, 0.05~0.1MPa of vacuum degree after 6~12h of pugging, aging 12~18h, hereafter repeats at room temperature
It is multiple to state operation, obtains the pug.
Further, in the step S4, the pug is put into extrusion shaping machine, be shaped to multichannel tubulose biscuit or
Tabular biscuit.
Preferably, the step S5 includes：
The biscuit is placed in room temperature environment dry 4~12h by S51, and the room temperature environment is 20~30 DEG C of temperature, phase
To humidity 50%~70%；
Biscuit after drying at room temperature is kept the temperature 1~3h by S52 under 100~150 DEG C of temperature condition；
Dried biscuit is placed in vacuum sintering furnace and is burnt by S53, and 1~3h is kept the temperature at 800~1000 DEG C,
Hereafter continue to be heated to 2100~2300 DEG C, and keep the temperature 1~3h, obtain the multichannel silicon carbide ceramic support body.
The multichannel silicon carbide ceramic support body of embodiment according to a second aspect of the present invention, according to above-described embodiment
The preparation method of multichannel silicon carbide ceramic support body be made.
Further, the porosity of the multichannel silicon carbide ceramic support body is 35%~45%, the contact with water
Angle is about 0.3 °, and bending strength is more than 80MPa.
The above-mentioned technical proposal of the present invention one of at least has the advantages that：
(1) in the preparation of supporter, coordinated by two kinds of silicon carbide powders of thickness, be on the one hand conducive to obtained by raising
Multichannel silicon carbide ceramic support body intensity, while advantageously reduce the sintering temperature of supporter, meanwhile, by using carbon
High-throughput multichannel silicon carbide ceramic support body can be made in primary raw material of the SiClx powder as supporter；
(2) according to above-mentioned multichannel silicon carbide ceramic support body, the angle of wetting of silicon carbide ceramics and water is only 0.3 °, table
It is now stronger hydrophilic and oleophobic characteristic；Good mechanical performance, bending strength are more than 80MPa；Porosity is 35%~45%
Between, with reference to its hydrophilic and oleophobic characteristic, the flux of silicon carbide ceramics membrane component prepared therefrom is up to 5 times of alumina ceramic membrane
More than；The chemical stability of silicon carbide is stronger, can be applied in the acid or alkali environment of pH=0~14, is resistant to various solvents and various
Concentration oxidizer.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of the multichannel silicon carbide ceramic support body of the embodiment of the present invention；
Fig. 2 is the microscopic appearance figure of multichannel silicon carbide ceramic support body being prepared according to the embodiment of the present invention 1；
Fig. 3 is the microscopic appearance figure of multichannel silicon carbide ceramics membrane component being prepared according to the embodiment of the present invention 1.
Specific embodiment
Purpose, technical scheme and advantage to make the embodiment of the present invention are clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill
Personnel's all other embodiments obtained, shall fall within the protection scope of the present invention.
Multichannel silicon carbide ceramic support body according to embodiments of the present invention is specifically described with reference to attached drawing first below
Preparation method.
As shown in Figure 1, the preparation method of multichannel silicon carbide ceramic support body according to embodiments of the present invention, including：
S1, according to mass ratio 100:(5~10)：(3~5):(10~15) weigh carborundum powder I, carborundum powder II, combine
Agent and pore creating material.
Wherein it is preferred to the average particle size range of carborundum powder I, between 35~55 μm, the carborundum powder II is put down
For equal particle size range between 0.5~3.0 μm, purity is more than 98%.
By the way that two kinds of silicon carbide powders of thickness are coordinated, higher-strength can be obtained at a relatively low sintering temperature
Pure silicon carbide supporter.Specific size about carborundum powder II is not particularly limited, it is contemplated that its usage amount, manufacture cost
Deng preferably the average particle size range of carborundum powder II is between 0.5~3 μm.In addition, about carborundum powder I and carborundum powder II
Mass ratio, without special provision, it is contemplated that comprehensive cost, the overall porosity of prepared supporter, supporter intensity, sintering
The factors such as temperature, preferred mass ratio are 100:(5~10).
Bonding agent can be selected from sodium carboxymethylcellulose, sodium hydroxyethlcellulose, methylcellulose, polyvinyl alcohol, poly- third
Olefin(e) acid etc. and its mixture.Wherein, preferably sodium carboxymethylcellulose, viscosity is preferably 10000~20000PaS, more excellent
Substantially 16000PaS is selected as, purity is more than 98.5%.In addition, the content about bonding agent, can combine used knot
The type of mixture, carborundum powder I and the grain size of carborundum powder II and proportioning situation etc. are set, the carbonization of preferably 100 mass parts
Silica flour I uses the bonding agent of 3~5 mass parts.
Pore creating material can be carbon black, activated carbon powder, corn flour or graphite powder, between average grain diameter is 5~10 μm.About making
The size and content of hole agent can combine porosity, used carborundum powder I and the carborundum powder of the supporter to be generated
II grain size and proportioning situation etc. are set, between preferably average grain diameter is 5~10 μm, and the carborundum powder I of 100 mass parts
Use the pore creating material of 10~15 mass parts.
The bonding agent is dissolved in water by S2, and carborundum powder I, carborundum powder II and the pore creating material are added in the knot
In the aqueous solution of mixture, mixed material is mixed to get, solid content is 50%~70%.
Specifically, for example, bonding agent sodium carboxymethylcellulose (CMC) stirring is dissolved in warm water, then warm water stirring, until
Bonding agent is completely dissolved；Again by the carborundum powder I of precise in step 1, carborundum powder II, carbon black, sodium carboxymethylcellulose
(CMC) solution sequentially adds mixing tank, is uniformly mixed that mixed material is made with high speed mixer.
By being mixed the carborundum powder of different-grain diameter and passing through addition bonding agent, mixed material can be effectively improved
In solid content, to improve the intensity of biscuit, further also advantageously improve the intensity of sintered supporter.
S3 is kneaded the mixed material in step S2, obtains pug.
Specifically, the mixed material in step S2 is put into vacuum deairing machine, in 0.08~0.12MPa of extrusion pressure,
Under conditions of 0.05~0.1MPa of vacuum degree after 6~12h of pugging, aging 12~18h at room temperature, hereafter repeatedly aforesaid operations are more
It is secondary, obtain pug.
The pug is carried out extrusion molding, obtains biscuit by S4.
Preferably, pug is put into vacuum extruding form machine, extrusion pressure can be 0.5~0.8MPa, and molding obtains more
Conduit tubular biscuit or tabular biscuit.
By changing extrusion die, tubular type or flat biscuit can be molded and made pottery with preparing corresponding multichannel silicon carbide
Porcelain film support.
About tubular type, such as the multichannels tubular type silicon carbide ceramic support body biscuit such as plastic 19 hole, 31 holes, 37 holes,
Its corresponding specification for example can be respectively(outer diameter × length),
About silicon carbide ceramics flat membrane support biscuit flat, such as that 43 holes, 50 holes, 80 holes can be molded.
S5 is burnt into after the biscuit is dried, obtains multichannel silicon carbide ceramic support body.
Preferably, step S5 includes the following steps：
The biscuit is placed in room temperature environment dry 4~12h by S51, and the room temperature environment is 20~30 DEG C of temperature, phase
To humidity 50%~70%；It can also be dried using forced ventilation；Or biscuit is placed in after drying at room temperature and moves into microwave and does
It is carried out in dry device dry at a high speed.
Biscuit after drying at room temperature is kept the temperature 1~3h by S52 at 100~150 DEG C.
Dried biscuit is placed in vacuum sintering furnace and is burnt by S53, and 1~3h is kept the temperature at 800~1000 DEG C,
Hereafter continue to be heated to 2100~2300 DEG C, and keep the temperature 1~3h, obtain the multichannel silicon carbide ceramic support body.
The multichannel silicon carbide ceramic support body has the characteristic of high intensity, and porosity is 35%~45%, with water
Contact angle for 0.3 °, bending strength is more than 80MPa.
The multichannel silicon carbide ceramics membrane element based on above-mentioned multichannel silicon carbide ceramic support body is detailed below
The preparation method of part.
The preparation method of multichannel silicon carbide ceramics membrane component, including：
(1) preparation of the preparation of supporter, wherein supporter is the system of above-mentioned multichannel silicon carbide ceramic support body
It is standby, then details are not described herein.
(2) preparation of transition zone, specifically includes following steps：
Step 21, according to mass ratio 100：(20~40)：(10~20) weigh carborundum powder III, polyvinyl alcohol and polypropylene
Acid；Wherein, the average particle size range of carborundum powder III is between 1~10 μm, preferably between 3~5 μm.
Preferably, the molecular weight of the polyvinyl alcohol is 2000, and purity is more than 99%, the molecular weight of the polyacrylic acid
It is 72.06, purity is more than 99%.
Step 22, above-mentioned material with water is mixed, obtains transition zone slurry, solid content is 30%~50%, preferably
40%.
Preferably, by the material and water by planetary ball mill, using the silicon ball that is carbonized as abrasive media, ball milling 5~
10h obtains the transition zone slurry.
Step 23, the supporter that step 15 obtains is placed in the transition zone slurry, makes the transition zone slurry in institute
10~20s of flowing in supporter is stated, flow velocity is 0.5~2m/s, and preferably flow velocity is 1m/s, in the endoporus table of the supporter
Face forms coating.Since this coating method is to form film layer in bore area, all it is unfavorable for shape when flow velocity is too high or too low
Into complete and uniform film layer.
Step 24, after bore area being formed with the supporter drying of coating, 1 is kept the temperature at 2000~2100 DEG C of temperature
~3h is sintered, to form transition zone in the bore area of the supporter.
(3) preparation of superficial film, specifically includes following steps：
Step 31, according to mass ratio 100：(15~25)：(5~10) weigh carborundum powder IV, polyvinyl alcohol and polypropylene
Acid.
Preferably, the average grain diameter of carborundum powder IV is 0.1~1 μm, and purity is more than 99%, point of the polyvinyl alcohol
Son amount is 2000, and purity is more than 99%, and the molecular weight of the polyacrylic acid is 72.06, and purity is more than 99%.
Step 32, above-mentioned material with water is mixed, obtains coating liquid, solid content is 25%~45%, preferably 35%.
Preferably, it into material plus after deionized water, is put into planetary ball mill, using the silicon ball that is carbonized as grinding medium
Matter, high speed 5~10h of ball milling, be made high stable, high solids content coating liquid.
Step 33, the supporter is placed in the coating liquid, the coating liquid is made to flow 10 in the supporter
~20s, flow velocity is 0.5~2m/s, preferably 1.2m/s, to form film on the transition zone.
Step 34, after being formed with the supporter drying of film, 1~2h of heat preservation is burnt at 1800~2000 DEG C of temperature
Knot, to form superficial layer on the transition zone.
Step 35, the supporter for being formed with superficial layer is placed in oxidation furnace and kept the temperature at 1000~1200 DEG C of temperature
1~3h carries out the oxidation processes, to obtain the superficial film of high-hydrophilic silicon carbide.
Specifically, the film thickness of obtained membrane component is 40~100 μm, and average pore size is 0.04~5 μm, preferably film thickness
0.7 μm of hydrophily silicon carbide film layer.Due to have passed through oxidation processes, reach 0.3 ° or so with the contact angle of water, have
High hydrophily.
By the above method, finally multichannel silicon carbide ceramic membrane element porosity obtained is 35%~45%, with water
Contact angle is 0.3 °, and bending strength is more than 80MPa.Compared with the membrane of oxide ceramics such as aluminium oxide, zirconium oxide, silicon carbide ceramics
The porosity higher of film, membrane flux bigger, high mechanical strength, chemical stability (pH ranges 0~14) is excellent, heat-resisting quantity is stronger
And cost performance is excellent.
Technical research personnel to enable this field are better understood from technical scheme of the present invention, with reference to example pair
The present invention is described in further detail.
The preparation of 1 silicon carbide ceramic support body 1 of embodiment
A1 weighs raw material：Bonding agent uses sodium carboxymethylcellulose (viscosity 16000PaS), and pore creating material uses carbon black,
By the carborundum powder I of 40 μm of grain size, carborundum powder II, sodium carboxymethylcellulose, the carbon black in mass ratio 100 of 0.5 μm of grain size:7:
4:12 weigh；
B1 raw materials mix：The sodium carboxymethylcellulose weighed in A1 stirring is dissolved in 40 DEG C of warm water, then successively first
Carborundum powder I, carborundum powder II and carbon black are added in, and is uniformly mixed with high speed mixer；
C1 raw materials are kneaded：Said mixture material is added in into vacuum deairing machine batch mixing 8h, vacuum degree 0.08MPa repeatedly；It is aging
16h；It repeats above operation, reaches pugging duration 16 hours, aging 32 hours；Extrusion pressure to be achieved (operating pressure during pugging
0.08~0.12MPa) after, it is squeezed out；
D1 supporter biscuit extrusion moldings：Pug in step C1 is put into vacuum extruding form machine, extrusion pressure
0.7MPa, molding obtain multichannel silicon carbide supporter biscuit；
E1 supporters biscuit is dried：The supporter biscuit of extrusion molding is placed in natural drying at room temperature；
If (November of Northern Part of China~April) in winter, workshop temperature is less than 20, the relative humidity of air
Less than 50%, supporter is easily dry and cracked, is not easy to spontaneously dry, and in order to avoid dry and cracked situation occurs in supporter, can will be extruded into
After the supporter of type is placed in room temperature (20 DEG C of temperature or more, relative humidity are more than 50%) natural drying 8 minutes, by simply divulging information
Pipe pressure is passed through warm wind and is dried.If workshop temperature is less than between 20, need to reach inlet air requirement, wind by air heating
Speed is controlled in 13m/s, when the relative humidity of workshop is less than 50%, can pass through the relative humidity that humidifier adjusts air
More than 50%；
F1 supporters biscuit is dried：Supporter biscuit enters drying oven after drying at room temperature, is slowly warming up to from room temperature through 3h
130 DEG C, keep the temperature 1h；Then Temperature fall；
G1 supporters are burnt into：The supporter that step F1 is completed to drying is packed into vacuum sintering furnace, and set temperature is raised to 800 DEG C
After keep the temperature 2h, then proceed to be warming up to 2300 DEG C, soaking time 4h, multichannel silicon carbide supporter 1 be made.Fig. 2 shows it
Microscopic appearance, the supporting body structure obtained as shown in Figure 2 are uniform.
The porosity of multichannel silicon carbide ceramic support body 1 is 45%, and the contact angle with water is 0.3 °, and bending strength is
83MPa。
Further, since the wetability of silicon carbide and water is relatively good, the ceramic supporting body prepared using carborundum powder is in Shui Chu
With larger flux, substantially the 5 of alumina support times during reason.
The preparation of 2 silicon carbide ceramics membrane component of embodiment
The multichannel silicon carbide supporter 1 obtained using embodiment 1, further prepares silicon carbide ceramics membrane component.
The preparation of transition zone
A2 is by the carborundum powder III, polyvinyl alcohol, polyacrylic acid in mass ratio 100 of 5 μm of grain size:20:12 precises；
B2 is put into the above-mentioned material weighed plus after deionized water in planetary ball mill, using the silicon ball that is carbonized as grinding medium
Matter, high speed ball milling 1.5h, obtained high stable, solid content are up to the transition zone slurry of 40% high solids content；
Slurry made from step B2 is moved into size barrel by C2, and slurry is injected into self-control coating device by drainage pump, is controlled
Flowing time control is in 12s in the Multichannel ceramic membrane supporter that slurrying material is obtained in embodiment 1, thus in supporter endoporus table
Face forms transition zone；
D2 moves into vacuum sintering furnace, sintering temperature after surface made from step C2 to be formed with to the supporter drying of transition zone
2100 DEG C, soaking time 1h, so as to prepare fine and close, uniform silicon carbide intermediate layer in silicon carbide supporting body surface.
The preparation of superficial film
A3 is by the carborundum powder IV, polyvinyl alcohol, polyacrylic acid in mass ratio 100 of 1 μm of grain size:20:8 precises；
B3 is put into the above-mentioned material weighed plus after deionized water in planetary ball mill, using the silicon ball that is carbonized to grind
High stable is made, the coating liquid for the high solids content that solid content is 35% in grinding media, high speed ball milling 1.5h；
Coating liquid made from step B3 is moved into size barrel by C3, and coating liquid is injected into self-control film by drainage pump fills
It puts, flowing time control is in 12s in multichannel supporter endoporus for coating liquid, so as to form film layer in supporter bore area；
D3 moves into vacuum sintering furnace, sintering temperature 1 after surface made from step C3 to be formed with to the supporter drying of film layer
900 DEG C, soaking time 1h, so as to prepare fine and close, uniform silicon carbide film layer in silicon carbide supporting body surface；
The supporter that silicon carbide film layer is coated with made from step D3 is placed in oxidation furnace, 1100 DEG C of oxidizing temperature, heat preservation by E3
Time 1h, so as to obtain the silicon carbide film layer of high-hydrophilic.
The microstructure of final multichannel silicon carbide ceramics membrane component obtained is shown in Fig. 3, porosity 40%, with water
Contact angle is 0.3 °, bending strength 90MPa.
The preparation of 3 silicon carbide ceramic support body 2 of embodiment
Become outside the pale of civilization except following, remaining process is the same as embodiment 1.
Multichannel silicon carbide ceramic support body prepare in, bonding agent select sodium hydroxyethlcellulose (viscosity for
18000PaS), the active powdered carbon of pore creating material selection, wherein, carborundum powder I (average grain diameter is 50 μm), carborundum powder II are (average
Grain size is 1 μm), methylcellulose and active powdered carbon be according to mass ratio 100:5:3:10 are weighed.
The final porosity that obtains is 43%, and the contact angle with water is 0.3 °, and bending strength is the multichannel silicon carbide of 87MPa
Ceramic film support 2.
Embodiment 4：
Become outside the pale of civilization except following, remaining process is the same as embodiment 1.
Multichannel silicon carbide ceramic support body prepare in, bonding agent select sodium carboxymethylcellulose (viscosity for
12000PaS), the active powdered carbon of pore creating material selection, carborundum powder I (average grain diameter is 35 μm), II (average grain diameter of carborundum powder
Be 3 μm), sodium carboxymethylcellulose and active powdered carbon be according to mass ratio 100:10:5:11.5 it is weighed.
The final porosity that obtains is 45%, and the contact angle with water is 0.3 °, and bending strength is the multichannel silicon carbide of 82MPa
Ceramic film support 3.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of multichannel silicon carbide ceramic support body, which is characterized in that include the following steps：
S1, according to mass ratio 100:(5~10)：(3~5):(10~15) weigh carborundum powder I, carborundum powder II, bonding agent and
Pore creating material, wherein, the average grain diameter of the carborundum powder I is more than the average grain diameter of the carborundum powder II；
The bonding agent is dissolved in water by S2, and carborundum powder I, carborundum powder II and the pore creating material are added in the bonding agent
Aqueous solution in, be mixed to get mixed material, solid content is 50%~70%；
S3 is kneaded the mixed material, obtains pug；
The pug is carried out extrusion molding, obtains biscuit by S4；
S5 is burnt into after the biscuit is dried, obtains multichannel silicon carbide ceramic support body.
2. the preparation method of multichannel silicon carbide ceramic support body according to claim 1, which is characterized in that the carbon
The average particle size range of SiClx powder I is between 35~55 μm, and the average particle size range of the carborundum powder II is at 0.5~3.0 μm
Between.
3. the preparation method of multichannel silicon carbide ceramic support body according to claim 1, which is characterized in that the step
In rapid S1, the bonding agent is selected from sodium carboxymethylcellulose, sodium hydroxyethlcellulose, methylcellulose, polyvinyl alcohol, polypropylene
Acid and its mixture.
4. the preparation method of multichannel silicon carbide ceramic support body according to claim 1, which is characterized in that the knot
Mixture is sodium carboxymethylcellulose, and viscosity is 10000~20000PaS.
5. the preparation method of multichannel silicon carbide ceramic support body according to claim 1, which is characterized in that the step
In rapid S1, the pore creating material is carbon black, activated carbon powder, corn flour or graphite powder, between average grain diameter is 5~10 μm.
6. the preparation method of multichannel silicon carbide ceramic support body according to claim 1, which is characterized in that the step
In rapid S3, the mixed material is put into vacuum deairing machine, in 0.08~0.12MPa of extrusion pressure, vacuum degree 0.05~
Under conditions of 0.1MPa after 6~12h of pugging, aging 12~18h at room temperature, hereafter repeatedly aforesaid operations are multiple, obtain described
Pug.
7. the preparation method of multichannel silicon carbide ceramic support body according to claim 1, which is characterized in that the step
In rapid S4, the pug is put into extrusion shaping machine, is shaped to multichannel tubulose biscuit or tabular biscuit.
8. the preparation method of multichannel silicon carbide ceramic support body according to claim 1, which is characterized in that the step
Rapid S5 includes：
The biscuit is placed in room temperature environment dry 4~12h by S51, and the room temperature environment is 20~30 DEG C of temperature, relatively wet
Degree 50%~70%；
Biscuit after drying at room temperature is kept the temperature 1~3h by S52 under 100~150 DEG C of temperature condition；
Dried biscuit is placed in vacuum sintering furnace and is burnt by S53,1~3h is kept the temperature at 800~1000 DEG C, hereafter
Continue to be heated to 2100~2300 DEG C, and keep the temperature 1~3h, obtain the multichannel silicon carbide ceramic support body.
9. a kind of multichannel silicon carbide ceramic support body, which is characterized in that pass through any one of claim 1 to 8 claim
The preparation method of the multichannel silicon carbide ceramic support body is made.
10. multichannel silicon carbide ceramic support body according to claim 9, which is characterized in that the multichannel carbonization
The porosity of silicon ceramic film support is 35%~45%, and the contact angle with water is 0.3 °, and bending strength is more than 80MPa.
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| CN109650935A (en) * | 2019-02-15 | 2019-04-19 | 中国计量大学 | A kind of preparation method of the adjustable alumina porous ceramic film of hole shape |
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| CN115745618A (en) * | 2022-11-21 | 2023-03-07 | 南京工业大学 | Method for improving mechanical strength of porous silicon carbide film |
| CN117142875A (en) * | 2022-05-23 | 2023-12-01 | 宁夏大学 | Porous gas slag-silicon carbide composite ceramic support and preparation method thereof |
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Application publication date: 20180710 |