CN108395252A - Liquid-phase sintering multichannel silicon carbide ceramic support body and preparation method thereof - Google Patents
Liquid-phase sintering multichannel silicon carbide ceramic support body and preparation method thereof Download PDFInfo
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- CN108395252A CN108395252A CN201810075180.8A CN201810075180A CN108395252A CN 108395252 A CN108395252 A CN 108395252A CN 201810075180 A CN201810075180 A CN 201810075180A CN 108395252 A CN108395252 A CN 108395252A
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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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The present invention provides liquid-phase sintering multichannel silicon carbide ceramic support body and preparation method thereof, and the preparation method of supporter includes：Carborundum powder I, kaolin, talcum, pore creating material and the first bonding agent are weighed, pug is configured to water and is molded, liquid-phase sintering multichannel silicon carbide ceramic support body is obtained through oversintering, wherein the sintering temperature of the supporter is 1500 DEG C or less.Due to, containing kaolin and talcum, sintering temperature being significantly reduced using liquid-phase sintering in the raw material of the supporter, meanwhile, the multichannel silicon carbide ceramic support body that kaolin, talcum and silicon carbide liquid phase sintering obtain has very high intensity.According to the multichannel silicon carbide ceramic support body that the present invention obtains, bending strength is more than 100MPa, and porosity can be applied in the acid or alkali environment of pH=0~14 between 35%~45%, be resistant to various solvents and various concentration oxidizers；Temperature in use can reach 800~1000 DEG C.
Description
Technical field
The present invention relates to the preparing technical fields of ceramic material, and in particular, to a kind of liquid-phase sintering multichannel silicon carbide
Ceramic film support 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 be typically derived from mining, metal smelt and processing, plating, process hides, pesticide, papermaking, paint,
The industries such as printing and dyeing, nuclear technology and petrochemical industry, contained heavy metal ion are difficult to biodegradable and are easily enriched with by bio-absorbable, poison
Property there is duration, be the pollutant of a kind of great potential hazard.
Currently, the method for heavy metal containing wastewater treatment can be substantially divided into three categories：(1) method of chemical treatment, i.e., weight in waste water
The method that metal ion is removed by the way that chemical reaction occurs；(2) physical treatment process makes the heavy metal ion in waste water not change
The method adsorbed under conditions of its chemical form, concentrate, detached；(3) biological treatment, by the wadding of microorganism or plant
The method that the effects that solidifying, uptake and accumulation, enrichment removes heavy metal ions in wastewater.But these methods are all different degrees of in practice
That there is treatment process on ground is longer, cost is higher, waste residue is more, introduce secondary pollution, treatment conditions are harsh, treating capacity is limited etc.
Problem.
The environment protectment protection being gradually increased in face of China, researcher are increasingly biased to handle weight using membrane separation technique
Metallic wastewater.In many seperation films, inorganic ceramic membrane is the important component of high performance membrane material, is by inorganic metal oxygen
What compound was prepared has the thin-film material for efficiently separating function, has high temperature resistant, resistance to chemical attack, mechanical strength good, anti-
Microorganism ability is strong, permeation flux is big, clanability is strong, pore-size distribution is narrow, service life is long, the advantage being hardly damaged etc..
The research of inorganic ceramic membrane at present is concentrated mainly on the membrane materials such as aluminium oxide, zirconium oxide, cordierite, commercialized inorganic
Ceramic membrane is mainly pellumina.However, the characteristics of heavy metal wastewater thereby, is deep-etching, oil-containing, contains heavy metal ion.So tight
Under cruel use environment, the strong acid-base resistance corrosive power of alumina ceramic membrane is weak, therefore service life is low, the membrane material update cycle
It is short；In addition, the angle of wetting of alumina ceramic membrane and pure water is about 30 °, therefore filtration flux is small, waste water treatment efficiency is low.
On the other hand, it although carbofrax material has that angle of wetting is small, mechanical strength is high etc. a little, is typically carbonized
The sintering temperature of silicon materials is higher, to it is high there are manufacturing cost the shortcomings of.
For this reason, it is necessary to research and develop, a kind of filtration flux is big, waste water treatment efficiency is high, service life is long, manufacturing cost
Low inorganic ceramic film support.
Invention content
In view of this, the present invention proposes a kind of preparation of the multichannel silicon carbide ceramic support body using liquid-phase sintering
Method, and multichannel silicon carbide ceramic membrane branch made from preparation method by above-mentioned multichannel silicon carbide ceramic support body
Support body.
In order to solve the above technical problems, present invention employs following technical schemes：
The preparation method of the liquid-phase sintering multichannel silicon carbide ceramic support body of embodiment according to a first aspect of the present invention,
Include the following steps：Weigh carborundum powder I, kaolin, talcum, pore creating material and the first bonding agent, with water be configured to pug and at
Type obtains liquid-phase sintering multichannel silicon carbide ceramic support body through oversintering, wherein sintering temperature is 1500 DEG C or less.
According to some embodiments of the present invention, the preparation of the supporter specifically comprises the following steps：
Step 11, according to mass ratio 100:(5~10)：(3~5):(5~15)：(5~10) weigh carborundum powder I, kaolinite
Soil, talcum, pore creating material and the first bonding agent, the average particle size range of the carborundum powder I is between 20~60 μm；
Step 12, first bonding agent is dissolved in water, carborundum powder I, kaolin, talcum and the pore creating material is added
Enter into the aqueous solution of first bonding agent, be mixed to get mixed material, solid content is 50%~70%；
Step 13, the mixed material is kneaded, obtains pug；
Step 14, the pug is subjected to extrusion molding, obtains biscuit；
Step 15, it is burnt into after the biscuit being dried, obtains the liquid-phase sintering multichannel silicon carbide ceramic membrane branch
Support body.
Further, in the step 13, 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 pugging 6~12 hours, aging 12~18 hours at room temperature, hereafter
It is multiple to repeat aforesaid operations, obtains the pug.
Further, in the step 14, the pug is put into extrusion shaping machine, is shaped to multichannel tubulose biscuit or flat
Plate biscuit.
Further, the step 15 may include：
Step 151, the biscuit is placed in room temperature environment it is 4~12 hours dry, the room temperature environment be temperature 20~
30 DEG C, relative humidity 50%~70%；
Step 152, the biscuit after drying at room temperature is kept the temperature to 1~3h at 100~150 DEG C；
Step 153, it will be burnt into the biscuit merging sintering furnace after drying, 1~3h kept the temperature at 800~1000 DEG C,
Hereafter continue to be heated to 1300~1500 DEG C, and keep the temperature 1~3h, obtain the liquid-phase sintering multichannel silicon carbide ceramic membrane support
Body.
According to some embodiments of the present invention, the pore creating material is carbon black, activated carbon powder or graphite powder, average grain diameter 5
Between~10 μm；First bonding agent is selected from sodium carboxymethylcellulose, sodium hydroxyethlcellulose, methylcellulose, polyethylene
Alcohol, polyacrylic acid and its mixture.
Preferably, first bonding agent be sodium carboxymethylcellulose, and the viscosity of first bonding agent be 10000~
20000Pa·S。
The liquid-phase sintering multichannel silicon carbide ceramic support body of embodiment according to a second aspect of the present invention, passes through above-mentioned
The preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body described in one embodiment is made.
Preferably, porosity be 35%~45%, substantially 0.3 ° of the contact angle with water, bending strength be 100MPa with
On.
The above-mentioned technical proposal of the present invention one of at least has the advantages that：
(1) supporter is prepared using the liquid-phase sintering effect of kaolin and carborundum powder, sintering temperature can be significantly reduced
Degree；
(2) use liquid-phase sintering multichannel silicon carbide ceramic support body intensity made from lqiuid phase sintering method high；
(3) multichannel carbon can be further made in multichannel silicon carbide ceramic support body according to the ... of the embodiment of the present invention
SiClx ceramic membrane element, in the multichannel silicon carbide ceramics membrane component, the wetability of silicon carbide ceramic membrane and water is preferable, shows as
Stronger hydrophilic and oleophobic characteristic；Good mechanical performance, bending strength are more than 100MPa；Prepared ceramic membrane element hole
Rate is between 35%~45%, and in conjunction with its hydrophilic and oleophobic characteristic, membrane flux reaches 3 times of alumina ceramic membrane or more；Silicon carbide
Chemical stability it is stronger, can be applied in the acid or alkali environment of pH=0~14, be resistant to various solvents and various concentration oxidizers；
Temperature in use can reach 800~1 000 DEG C.
Description of the drawings
Fig. 1 be the embodiment of the present invention liquid-phase sintering multichannel silicon carbide ceramic membrane part making method in supporter system
Standby flow chart；
The microscopic appearance figure of liquid-phase sintering multichannel silicon carbide ceramic support body prepared by Fig. 2 present examples 1；
Fig. 3 is the photo of the liquid-phase sintering multichannel silicon carbide ceramics membrane component prepared by present example 1；
Fig. 4 is the SEM photograph of the liquid-phase sintering multichannel silicon carbide ceramic membrane element cross-section prepared by present example 1.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention 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 a part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill
The every other embodiment that personnel are obtained, shall fall within the protection scope of the present invention.
The preparation of multichannel silicon carbide ceramic support body according to the ... of the embodiment of the present invention is specifically described below in conjunction with the accompanying drawings
Method.
The preparation method of multichannel silicon carbide ceramic support body according to the ... of the embodiment of the present invention, weighs carborundum powder first
I, kaolin, talcum, pore creating material and the first bonding agent, are configured to pug with water by above-mentioned material and are molded, then, at 1500 DEG C
Through oversintering at temperature below, multichannel silicon carbide ceramic support body is obtained.
In detail, as shown in Figure 1, liquid-phase sintering multichannel silicon carbide ceramic support body according to the ... of the embodiment of the present invention
Preparation method, including：
Step 11, according to mass ratio 100:(5~10)：(3~5):(5~15)：(5~10) weigh carborundum powder I, kaolinite
Soil, talcum, pore creating material and the first bonding agent.
Wherein it is preferred to which the average particle size range of the carborundum powder I, between 20~60 μm, purity is 98% or more.
First bonding agent can be selected from sodium carboxymethylcellulose, sodium hydroxyethlcellulose, methylcellulose, polyethylene
Alcohol, polyacrylic acid etc. and its mixture.Preferably, first bonding agent be carboxymethyl cellulose or sodium carboxymethylcellulose,
Its viscosity is preferably 10000~20000PaS, more preferably substantially 16000PaS, and purity is 98.5% or more.
The pore creating material can be carbon black, activated carbon powder or graphite powder, between average grain diameter is 5~10 μm.
Step 12, first bonding agent is dissolved in water, and carborundum powder I, kaolin, talcum and the pore creating material are added
Into the aqueous solution of first bonding agent, it is mixed to get mixed material, solid content is 50%~70%.
Specifically, for example, the stirring of the first bonding agent sodium carboxymethylcellulose (CMC) is dissolved in warm water, then warm water is stirred
It mixes, until bonding agent is completely dissolved；Again by the carborundum powder I of precise in step 11, kaolin, talcum, carbon black (pore creating material),
Sodium carboxymethylcellulose (CMC) solution sequentially adds mixing tank, is uniformly mixed with high speed mixer mixed material is made.
Step 13, the mixed material in step 12 is kneaded, obtains pug.
Specifically, the mixed material in step 12 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 pugging 6~12 hours, aging 12~18 hours at room temperature, hereafter repeat above-mentioned
Operation is multiple, obtains pug.
Step 14, the pug is subjected to extrusion molding, obtains biscuit.
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 the multichannels tubular type silicon carbide ceramic support body biscuit such as tubular type, such as plastic 19 hole, 31 holes, 37 holes,
Its corresponding specification is respectively(outer diameter × length),
About silicon carbide ceramics flat membrane component flat, such as that 43 holes, 50 holes, 80 holes can be molded.
Step 15, it is burnt into after the biscuit being dried, obtains liquid-phase sintering multichannel silicon carbide ceramic support body.
Preferably, step 15 includes the following steps：
Step 151, the biscuit is placed in room temperature environment it is 4~12 hours dry, the room temperature environment be temperature 20~
30 DEG C, relative humidity 50%~70%.
It can also be dried using forced ventilation；Or biscuit is placed in after drying at room temperature to move into microwave dryer and is carried out
High speed is dry.
Step 152, the biscuit after drying at room temperature is kept the temperature to 1~3h at 100~150 DEG C.
Step 153, it will be burnt into the biscuit merging sintering furnace after drying, 1~3h kept the temperature at 800~1000 DEG C,
Hereafter continue to be heated to 1300~1500 DEG C, and keep the temperature 1~3h, obtain the liquid-phase sintering multichannel silicon carbide ceramic membrane support
Body.
Due to having used kaolin and talcum in raw material, using it in sintering process lower fusing point, burnt using liquid phase
Knot technology significantly reduces the sintering temperature of silicon carbide ceramics.
In addition, the multichannel silicon carbide ceramic support body obtained by liquid-phase sintering, the characteristic with high intensity,
Porosity is 35%~45%, smaller with the contact angle of water, and bending strength is 100MPa or more.
Liquid-phase sintering multichannel silicon carbide ceramic support body according to the ... of the embodiment of the present invention, can be used for preparing multichannel
Silicon carbide ceramics membrane component.Specifically, further it was arranged on the liquid-phase sintering multichannel silicon carbide ceramic support body
Layer and superficial film are crossed to prepare.
The preparation process of transition zone and superficial film is as follows：
The preparation of transition zone, specifically includes following steps：
Step 21, according to mass ratio 100：(10~20)：(10~20)：(3~5) weigh carborundum powder II, kaolin,
Two bonding agents and the first dispersant, the average particle size range of the carborundum powder II between 2~20 μm, purity be 98% with
On.
Second bonding agent can be selected from sodium carboxymethylcellulose, sodium hydroxyethlcellulose, methylcellulose, polyethylene
Alcohol, polyacrylic acid and its mixture.Wherein, second bonding agent is preferably polyvinyl alcohol, the molecular weight of the polyvinyl alcohol
It is 2000, purity is 99% or more.
First dispersant can be selected from polyacrylic acid, ammonium citrate, methylcellulose, polyethylene glycol, poly- methyl-prop
Olefin(e) acid ammonium and its mixture.Wherein, first dispersant is preferably polyacrylic acid, and the molecular weight of the polyacrylic acid is
72.06, purity is 99% or more.
Step 22, above-mentioned material is mixed with water, obtains transition zone slurry, solid content is 30%~50%, preferably
40%.
Preferably, the material and water are passed through into planetary ball mill, using the silicon ball that is carbonized as abrasive media, 5~10h of ball milling
Hour, obtain 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 being formed completely when flow velocity is too high or too low
And uniform film layer.
Step 24, it is sintered after bore area being formed with to the supporter drying of coating, in the supporter
Bore area forms transition zone.Preferably, the sintering can be carried out by 1~3h of heat preservation at 1200~1400 DEG C of temperature.
Similarly, by containing kaolin, also, the grain size by reducing silicon carbide powder in the raw material of transition zone,
Effectively further reduce sintering temperature.
The preparation of superficial film, specifically includes following steps：
Step 31, according to mass ratio 100：(15~25)：(5~10) weigh carborundum powder III, third bonding agent and second
Dispersant.
Preferably, for the average particle size range of the carborundum powder III between 0.1~2 μm, purity is 98% or more.
The third bonding agent can be selected from sodium carboxymethylcellulose, sodium hydroxyethlcellulose, methylcellulose, polyethylene
Alcohol, polyacrylic acid and its mixture.Wherein, the third bonding agent is preferably polyvinyl alcohol, the molecular weight of the polyvinyl alcohol
It is 2000, purity is 99% or more.
Second dispersant can be selected from polyacrylic acid, ammonium citrate, methylcellulose, polyethylene glycol, poly- methyl-prop
Olefin(e) acid ammonium and its mixture.Wherein, second dispersant is preferably polyacrylic acid, and the molecular weight of the polyacrylic acid is
72.06, purity is 99% or more.
It should be noted that above-mentioned first bonding agent, the second bonding agent, third bonding agent can be the same or different,
It is selected not by interfering with each other, that is to say, that it is selected from above-mentioned material independently from each other.
Similarly, above-mentioned first dispersant and the second dispersant can be the same or different, and selection is not done each other
It disturbs, that is to say, that it is selected from above-mentioned material independently from each other.
Step 32, above-mentioned material is mixed with water, 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
The coating liquid of high stable, high solids content is made in matter, high speed 5~10h of ball milling.
Step 33, the coating liquid is made to flow 10~20s in the supporter, flow velocity is 0.5~2m/s, preferably
1.2m/s, to form film on the transition zone.
For example, the supporter can be placed in the coating liquid or be placed in film applicator, while making coating liquid
It is flowed in the supporter with certain flow rate, to form film on the transition zone.Step 34, the support of film will be formed with
After body drying, 1~3h of heat preservation is sintered at 1100~1300 DEG C of temperature, to form superficial film on the transition zone.
Specifically, the film thickness of obtained membrane component is 40~100 μm, and average pore size is 0.04~1 μm, preferably 0.5 μ
The hydrophily silicon carbide film layer of m.The contact angle of the film layer and water reaches 0.3 ° or so, has high hydrophily.
By the above method finally liquid-phase sintering multichannel silicon carbide ceramic membrane element porosity obtained be 35%~
45%, for the contact angle with water close to 0.3 °, bending strength is 100MPa or more.With the membrane of oxide ceramics such as aluminium oxide, zirconium oxide
It compares, porosity higher, membrane flux bigger, high mechanical strength, the chemical stability (pH ranges 0~14) of silicon carbide ceramic membrane are excellent
It is different, heat-resisting quantity is stronger and cost performance is excellent.Silicon carbide ceramic membrane and smaller ° of the angle of wetting of water, therefore silicon carbide ceramic membrane has
There are high hydrophily and oil repellency.
To enable the technical research personnel of this field to be 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 liquid phase sintering silicon carbide ceramic film support of embodiment.
A1 weighs raw material：First bonding agent uses sodium carboxymethylcellulose, and pore creating material uses carbon black, by 40 μm of carbon of grain size
SiClx powder I, kaolin, talcum, sodium carboxymethylcellulose, carbon black in mass ratio 100:7:4:10:8 weigh.
B1 raw materials mix：The sodium carboxymethylcellulose weighed in A1 stirring is dissolved in 40 DEG C of warm water first, then successively
Carborundum powder I, kaolin, talcum and carbon black is added, is used in combination high speed mixer to be uniformly mixed, wherein solid content 62%.
C1 raw materials are kneaded：Said mixture material is added vacuum deairing machine batch mixing 8h repeatedly, extrusion pressure when pugging
0.10MPa, vacuum degree 0.08MPa；Aging 16h；Pugging on daytime again, it is aging at night, it is spare to obtain pug.
D1 supporter biscuits squeeze out：Pug in step C1 is put into vacuum extruding form machine, extrusion pressure 0.7MPa is squeezed
Go out the tubular type extruder head that mold is 19 holes, obtains 19 hole multichannel tubular type silicon carbide supporter biscuits.
E1 supporter biscuits are 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 DEG C, the relative humidity of air
Also below 50%, supporter is easily dry and cracked, is not easy to spontaneously dry.In order to avoid dry and cracked situation occurs in supporter, can will squeeze
Go out molding supporter to be placed in after room temperature (20 DEG C of temperature or more, relative humidity be more than 50%) spontaneously dries 8 minutes, by simple
Ventilation duct pressure is passed through warm wind and is dried.If workshop temperature be less than 20 DEG C, need by air carry out heating reach into
Wind requirement, blast velocity control is in 13m/s, when the relative humidity of workshop is less than 50%, can adjust air by humidifier
50% or more relative humidity.
F1 supporter biscuits are dried：Supporter enters drying oven after drying at room temperature, and 130 are slowly warming up to from room temperature through 3h
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 sintering furnace, and set temperature is protected after being raised to 800 DEG C
Warm 2h then proceedes to be warming up to 1400 DEG C, soaking time 2h, and it is liquid-phase sintering multichannel silicon carbide ceramic membrane that bending strength, which is made,
Supporter 1, microstructure is shown in Fig. 2.
The bending strength of liquid-phase sintering multichannel silicon carbide ceramic support body 1 is 110MPa.
The liquid-phase sintering multichannel silicon carbide supporter that embodiment 2 is obtained using embodiment 1 further prepares silicon carbide pottery
Porcelain membrane component.
The preparation of transition zone：
A2 by 5 μm of carborundum powders II of grain size, kaolin, as the polyvinyl alcohol of the second bonding agent, as the first dispersant
Polyacrylic acid in mass ratio 100:20:20:12 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 10h, obtained high stable, solid content are up to 40% transition zone slurry；
Slurry made from step B2 is moved into size barrel by C2, and slurry is injected into coating device, control slurry by drainage pump
Flowing time control is in 12s in the liquid-phase sintering Multichannel ceramic membrane supporter that embodiment 1 obtains for material, in supporter
Hole surface forms transition zone；
D2 moves into sintering furnace, sintering temperature 1300 after surface made from step C2 to be formed with to the supporter drying of transition zone
DEG C, soaking time 1h, to prepare fine and close, uniform silicon carbide intermediate layer in silicon carbide supporting body surface.
The preparation of superficial film：
A3 is by grain size 0.5 μm of carborundum powder III, polyvinyl alcohol, polyacrylic acid in mass ratio 100:20:8 precises；
B3 is put into the above-mentioned material weighed plus after deionized water in planetary ball mill, is to grind with the silicon ball that is carbonized
High stable is made, the coating liquid that solid content is 35% in grinding media, high speed ball milling 8h；
Coating liquid made from step B3 is moved into size barrel by C3, and coating liquid is injected into coating device by drainage pump, is applied
Flowing time control is in 12s in multichannel supporter endoporus for film liquid, to form film layer in supporter bore area；
D3 moves into sintering furnace, sintering temperature 1100 after surface made from step C3 to be formed with to the supporter drying of film layer
DEG C, soaking time 1h finally obtains porosity to prepare fine and close, uniform silicon carbide film layer in silicon carbide supporting body surface
It is 40%, for the contact angle with water close to 0.3 °, bending strength is the liquid-phase sintering multichannel silicon carbide ceramics membrane component of 120MPa
And its microstructure (with reference to figure 3 and Fig. 4).
The preparation of 3 liquid-phase sintering multichannel 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, the first 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), kaolin, talcum, carboxylic
Methylcellulose, active powdered carbon are according to mass ratio 100:8:3:10:10 are weighed, and solid content is in mixed slurry
67%.
In addition, sintering temperature is 1500 degrees Celsius, soaking time is 3 hours.
It is final to obtain the liquid-phase sintering multichannel silicon carbide ceramic support body 2 that bending strength is 124MPa.
The preparation of 4 liquid-phase sintering multichannel silicon carbide ceramic support body 3 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, the first bonding agent select sodium carboxymethylcellulose (viscosity for
12000PaS), the active powdered carbon of pore creating material selection, wherein carborundum powder I (average grain diameter is 30 μm), kaolin, talcum, carboxylic
Methylcellulose, active powdered carbon are according to mass ratio 100:5:5:15:5 are weighed, and solid content is 55% in mixed slurry.
In addition, sintering temperature is 1350 degrees Celsius, soaking time is 3 hours.
It is final to obtain the liquid-phase sintering multichannel silicon carbide ceramic support body 3 that bending strength is 105MPa.
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, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body, which is characterized in that include the following steps：
Carborundum powder I, kaolin, talcum, pore creating material and the first bonding agent are weighed, pug is configured to water and is molded, obtained through oversintering
To the liquid-phase sintering multichannel silicon carbide ceramic support body, wherein sintering temperature is 1500 DEG C or less.
2. the preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body according to claim 1, feature exist
In specifically comprising the following steps：
Step 11, according to mass ratio 100:(5~10)：(3~5):(5~15)：(5~10) weigh carborundum powder I, kaolin,
Talcum, pore creating material and the first bonding agent, the average particle size range of the carborundum powder I is between 20~60 μm；
Step 12, first bonding agent is dissolved in water, carborundum powder I, kaolin, talcum and the pore creating material is added to
In the aqueous solution of first bonding agent, it is mixed to get mixed material, solid content is 50%~70%；
Step 13, the mixed material is kneaded, obtains pug；
Step 14, the pug is subjected to extrusion molding, obtains biscuit；
Step 15, it is burnt into after the biscuit being dried, obtains the liquid-phase sintering multichannel silicon carbide ceramic support body.
3. the preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body according to claim 2, feature exist
In in the step 13, the mixed material being put into vacuum deairing machine, in 0.08~0.12MPa of extrusion pressure, vacuum degree
Under conditions of 0.05~0.1MPa after pugging 6~12 hours, aging 12~18 hours at room temperature, hereafter repeatedly aforesaid operations were more
It is secondary, obtain the pug.
4. the preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body according to claim 2, feature exist
In in the step 14, the pug is put into extrusion shaping machine, is shaped to multichannel tubulose biscuit or tabular biscuit.
5. the preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body according to claim 2, feature exist
In the step 15 includes：
Step 151, the biscuit being placed in drying 4~12 hours in room temperature environment, the room temperature environment is 20~30 DEG C of temperature,
Relative humidity 50%~70%；
Step 152, the biscuit after drying at room temperature is kept the temperature to 1~3h at 100~150 DEG C；
Step 153, it will be burnt into the biscuit merging sintering furnace after drying, 1~3h kept the temperature at 800~1000 DEG C, hereafter
Continue to be heated to 1300~1500 DEG C, and keep the temperature 1~3h, obtains the liquid-phase sintering multichannel silicon carbide ceramic support body.
6. the preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body according to claim 1, feature exist
In the pore creating material is carbon black, activated carbon powder or graphite powder, between average grain diameter is 5~10 μm.
7. the preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body according to claim 1, feature exist
In first bonding agent is selected from sodium carboxymethylcellulose, sodium hydroxyethlcellulose, methylcellulose, polyvinyl alcohol, polypropylene
Acid and its mixture.
8. the preparation method of liquid-phase sintering multichannel silicon carbide ceramic support body according to claim 7, feature exist
In first bonding agent is sodium carboxymethylcellulose, and the viscosity of first bonding agent is 10000~20000PaS.
9. a kind of liquid-phase sintering multichannel silicon carbide ceramic support body, which is characterized in that pass through any one of claim 1 to 8
The preparation method of the multichannel silicon carbide ceramic support body is made.
10. liquid-phase sintering multichannel silicon carbide ceramic support body according to claim 9, which is characterized in that porosity
It is 35%~45%, bending strength is 100MPa or more.
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