CN108911779A - Method for preparing porous silicon carbide ceramic tube at low temperature through extrusion molding - Google Patents
Method for preparing porous silicon carbide ceramic tube at low temperature through extrusion molding Download PDFInfo
- Publication number
- CN108911779A CN108911779A CN201811048791.XA CN201811048791A CN108911779A CN 108911779 A CN108911779 A CN 108911779A CN 201811048791 A CN201811048791 A CN 201811048791A CN 108911779 A CN108911779 A CN 108911779A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- extrusion molding
- porous silicon
- sintering
- carbide ceramic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000919 ceramic Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000001125 extrusion Methods 0.000 title claims abstract description 22
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004014 plasticizer Substances 0.000 claims abstract description 8
- 239000000314 lubricant Substances 0.000 claims abstract description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 31
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 26
- 239000012188 paraffin wax Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 11
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 10
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 229920000609 methyl cellulose Polymers 0.000 claims description 8
- 239000001923 methylcellulose Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 6
- -1 sintering aid Substances 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000004018 waxing Methods 0.000 claims description 2
- 208000037656 Respiratory Sounds Diseases 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 12
- 230000004907 flux Effects 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000000462 isostatic pressing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Press-Shaping Or Shaping Using Conveyers (AREA)
- Ceramic Products (AREA)
Abstract
The invention relates to a method for preparing a large-aperture porous silicon carbide ceramic tube at low temperature through extrusion molding. According to the method for preparing the porous silicon carbide support body at the low temperature based on CN 105884394, a ceramic pug with good plasticity is obtained by adding a lubricant, water and a plasticizer into ceramic powder, then vacuum pugging is carried out, extrusion molding and drying are carried out, and finally, the tubular porous silicon carbide ceramic support body is obtained by sintering at a low temperature of 1150 ℃. The invention matches the extrusion of different tube types with the plasticity index, has the advantages of high production efficiency and high yield, and the prepared ceramic tube has the advantages of higher strength, gas permeability and the like, and can be applied to the field of high-temperature gas-solid separation.
Description
Technical field
The present invention relates to a kind of methods of extrusion molding low-temperature preparation of porous silicon carbide ceramic, belong to porous ceramics preparation
Technical field.
Background technique
Silicon carbide ceramic membrane has preferable mechanical strength, and excellent corrosion resistance and antioxygenic property are ceramics
Material high temperature mechanical property（Anti-thermal shock, creep resistance）One of best material, being used as high-temperature smoke filter has uniqueness
Advantage.Silicon carbide ceramics problems faced is mainly higher cost caused by sintering temperature height at present；Production cycle is long, production
Low efficiency.Therefore sintering temperature is reduced, suitable production technology is selected, production efficiency is improved and is of great significance.
Research shows that sintering temperature can be effectively reduced by using reaction in-situ sintering, such as by addition sintering aid
Al2O3, Al2O3-Y2O3, ZrO2Deng the use neopelex of basic patent CN 105884394 and zirconium oxide conduct burning
Auxiliary agent is tied, sintering temperature is successfully reduced to 1150 DEG C.
In terms of production technology, common tubular ceramic forming technique has isostatic pressing, injection forming, extrusion molding
Deng, wherein isostatic pressing be suitable for suppress big part and elongated product, can arbitrarily adjust briquetting pressure, the product matter of compacting
Amount is high, and firing contraction is small, and blank is fine and close, is unlikely to deform.106588021 A of patent CN provides a kind of cold isostatic compaction preparation
The method of silicon carbide ceramics, it is characterised in that use partial size ratio for 200 μm：60 μm：15 μm：1 μm=0.55:0.2:0.2:
0.05 silicon carbide is aggregate, and green body is pressed at 220 MPa, and sintering obtains product at 1700 DEG C.But static pressure is waited to produce
It cannot continuously cause yield lower.Slip-casting shaping process is formed by plaster mold water suction method, easy to operate.Patent CN
107244920 A provide a kind of method of silicon carbide injection forming sintering, it is characterised in that using the silicon carbide of submicron order
Powder, with Al2O3And Y2O3For sintering aid, forms after aging 12 h of pug, be sintered at 1800 DEG C.But it is produced
Period is long, and it is larger that green body is burnt into contraction distortion, and upper lower wall thickness is easy to appear deviation, and production efficiency is lower, higher cost.And it squeezes
Forming out has many advantages, such as that productivity is higher compared with other forming techniques, can consecutive production.105461306 A of patent CN,
Partial size is used to carry out extrusion molding as aggregate for 40 μm of silicon carbide, product strength reaches 306 MPa in room temperature, due to trip
From silicon there are its corrosion resistance is poor.101560104 A of patent CN is related to the preparation method of a kind of carborundum tube or stick, adopts
It is aggregate with 0.5 μm of silicon carbide of partial size, sintering obtains 3.14 g/cm of density at 2100 DEG C3, 490 Mpa's of bending strength
Ceramics.It is influenced by raw material plasticity, the partial size that extrusion molding uses is all smaller, and the ceramic aperture of firing is less than normal to cause air flux ratio
It is smaller.Currently used for gas solid separation silicon carbide ceramic to prepare pertinent literature less.
Summary of the invention
It is an object of the present invention to provide a kind of methods that efficient extrusion molding prepares porous silicon carbide ceramic pipe；Based on CN
The formula of 105884394 low-temperature preparation of porous silicon carbide supporters prepares the support of different casts by adjusting plasticity index
Body, and the forming method has high-efficient, high yield rate in production, consume energy few advantage, and sintering temperature is low, the ceramics burnt
The advantages that finished product has structure uniform, and intensity is high, good penetrability.
Technical scheme is as follows：
A kind of method of extrusion molding low-temperature preparation of porous silicon carbide ceramic, includes the following steps,
（1）By silicon carbide, pore creating material, sintering aid, binder, which is placed in by a certain percentage in three-dimensional material mixer, mixes 12 ~ 24 h,
40 ~ 60 r/min of revolving speed；
（2）Plasticizer, lubricant, water are added in powder upon mixing, is stirred in high-speed mixer by a certain percentage
0.5 ~ 1h, 240 ~ 360 r/min of mixing speed；
（3）By wet feed made from step 2, vacuum pugging is carried out, the preferable mud column of plasticity is obtained；
（4）The mud column of plasticity made from step 3 is placed in extruder and carries out extrusion molding.
（5）The green compact that step 4 is obtained be put into baking oven according to different wall thickness be arranged distinct program dried, de-waxing, so
After be sintered.
The present invention is based on the formula of 105884394 low-temperature preparation of porous silicon carbide supporter of CN, the amplification being formulated and
Industrialized production.Step（1）The silicon carbide average grain diameter is 100 ~ 200 μm, and sintering aid selects zirconium oxide and dodecane
Base benzene sulfonic acid sodium salt, pore creating material are active powdered carbon, and partial size is 5 ~ 20 μm, and binder is methylcellulose, the quality percentage of each component
Than for silicon carbide：Sintering aid：Pore creating material：Binder=71 ~ 76：2~7：20:2.
Wherein step（2）The plasticizer is glycerol, and lubricant is paraffin；The mass percent of each substance is powder：
Water：Glycerol：Paraffin=100:10~12：1~5：1~5.
Step（3）Pugging condition is 0.08 ~ 0.09 MPa of vacuum degree, and pugging number 1 ~ 6 time, the mud column practised is without obviously splitting
Line.
Step（4）The extrusion condition is 6 ~ 12 MPa.
Step（5）The drying procedure is, after drying 4 h in baking oven at 40 DEG C, then 12 ~ 24 is dried at 80 DEG C
h；The de-waxing program is, 0 ~ 500 DEG C of heating rate is 0.5 ~ 2 DEG C/min, 500 DEG C of 2 h of heat preservation, sintering procedure for 500 ~
1000 DEG C of heating rates are 10 DEG C/min, and 1000 ~ 1150 DEG C of heating rate is 1 DEG C/min, after keeping the temperature 2 ~ 3 h at 1150 DEG C
Temperature fall obtains porous silicon carbide ceramic pipe.
The beneficial effects of the present invention are：
（1）The present invention, as sintering aid, can reduce the sintering temperature of supporter using zirconium oxide and neopelex
Degree；Neopelex has good surface-active, the modeling to pug as a kind of anionic surfactant simultaneously
Property has facilitation；By the way that the process optimizations ceramics molding effects such as plasticizer, lubricant and vacuum pugging are added, it is less prone to
The problems such as cracking picking.
（2）The present invention matches plasticity index and green compact, can efficiently prepare the ceramics of different tubuloses.Sintering obtains
Porous silicon carbide ceramic pipe have higher gas permeability and intensity, be satisfied with high-temperature gas-solid separation application.
Detailed description of the invention
Fig. 1 is carborundum porous ceramics preparation flow figure.
Fig. 2 is the different silicon carbide porous ceramic pipe types of extrusion molding preparation.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
The aggregate selected is d50=100 μm of silicon-carbide particle, pore creating material d50=20 μm of active powdered carbon, sintering aid are
d50=5 μm of zirconium oxide and neopelex, binder are methylcellulose, and plasticizer is glycerol, and lubricant is
Paraffin, the above raw material are all technical grades.
Mixing method is divided into two steps, and the first step is the mixing of powder, and three-dimensional material mixer is selected to be mixed.By silicon carbide：
Sintering aid：Active powdered carbon：Methylcellulose is 75 by mass percentage:4:20:2 are configured, and in three-dimensional material mixer
24 h of mixing are carried out, wherein sintering aid is made of neopelex and zirconium oxide, ratio 1:1.Second step is powder
The mixing of material and liquid selects blender to be mixed.Mixed powder is placed in blender, carries out liquid feeding while stirring,
The mass percent of powder and liquid is powder：Water：Glycerol：Paraffin=100:10:2:3, after liquid is added several times, filled
Divide stirring 2 h.
The wet feed being stirred is put into vacuum deairing machine and carries out pugging, the number of pugging is 6 times, vacuum degree 0.08
MPa obtains the preferable mud section of plasticity, and measuring its plasticity index is 0.8.Then mud section is placed in the pug cylinder of extruder,
It carries out squeezing out outer diameter under the constant pressure of 10 MPa being 40 mm, internal diameter is the green compact of 30 mm, and length can be according to requiring to intercept.
Green compact are placed in customized V-groove and are dried, drying procedure is 4 h at 40 DEG C, then 12 h at 80 DEG C.
Blank strength after drying is larger, facilitates carrying.The green body being baked is put into high-temperature electric resistance furnace and is sintered, 0 ~ 500 DEG C of liter
Warm rate is 2 DEG C/min, and 500 DEG C of 2 h of heat preservation, 500 ~ 1000 DEG C of heating rates are 10 DEG C/min, 1000 ~ 1150 DEG C of heating speed
Rate is 1 DEG C/min, and Temperature fall after 2 h is kept the temperature at 1150 DEG C.
The performance of gained supporter is as follows, and aperture is 34 μm, porosity 46%, and breaking load is 2055 N, air flux
For 151 m3/(m2·h·kPa)。
Embodiment 2
By silicon carbide:Sintering aid：Active powdered carbon：Methylcellulose is 71 by mass percentage:7:20:2 carry out configuration powder,
Wherein sintering aid is made of neopelex and zirconium oxide, ratio 2:5.The quality of powder, water, glycerol, paraffin
Percentage is 100:11:5:5, the wet feed being stirred is put into vacuum deairing machine and carries out pugging, the number of pugging is 6 times, very
Reciprocal of duty cycle is 0.09 MPa, obtains the preferable mud section of plasticity, and it is 0.6 that plasticity index is measured after pugging, by the mud section got in 8 MPa
Constant pressure under squeeze out 40 mm of outer diameter, the green compact of internal diameter 26 mm and 20 mm.Green compact are placed in customized V-groove and are dried,
Drying procedure is 4 h at 40 DEG C, 12 h at 80 DEG C.The heating rate that sintering procedure is 0 ~ 500 DEG C is 1 DEG C/min, 500 DEG C of heat preservations
2 h, 500 ~ 1000 DEG C of heating rates are 10 DEG C/min, and 1000 ~ 1150 DEG C of heating rate is 1 DEG C/min, is protected at 1150 DEG C
Temperature fall after 2 h of temperature.
The performance of gained supporter is as follows, and the aperture of 26 mm of internal diameter is 30 μm, and porosity 46%, breaking load is
3095 N, air flux are 130 m3/(m2HkPa), the aperture of 30 mm of internal diameter is 29 μm, and porosity 46% breaks load
For 4901 N, air flux is 117 m3/(m2·h·kPa)。
Embodiment 3
The aggregate selected is d50=100 μm and d50=200 μm of silicon carbide, mass percent 1:1.By silicon carbide:Sintering helps
Agent：Active powdered carbon：Methylcellulose is 74 by mass percentage:4:20:2 carry out configuration powder, and wherein sintering aid is by 12
Sodium alkyl benzene sulfonate and zirconium oxide composition, ratio 1:1.Powder, water, glycerol, paraffin mass percent be 100:12:1:1,
The wet feed being stirred is put into vacuum deairing machine and carries out pugging, the number of pugging is 6 times, and vacuum degree is 0.08 MPa, is obtained
The preferable mud section of plasticity, it is 0.7 that plasticity index is measured after pugging, and then the mud section got is placed in the pug cylinder of extruder,
40 mm of outer diameter is squeezed out under the constant pressure of 6 MPa, the green compact of 30 mm of internal diameter, length can be according to requiring to intercept.Green compact, which are placed on, to be ordered
It is dried in the V-groove of system, drying procedure is 4 h at 40 DEG C, 24 h at 80 DEG C.The heating speed that sintering procedure is 0 ~ 500 DEG C
Rate is 0.5 DEG C/min, and 500 DEG C of 2 h of heat preservation, 500 ~ 1000 DEG C of heating rates are 10 DEG C/min, 1000 ~ 1150 DEG C of heating rate
For 1 DEG C/min, Temperature fall after 2 h is kept the temperature at 1150 DEG C.
The performance of gained supporter is as follows, and aperture is 40 μm, porosity 47.2%, and breaking load is 1430 N, and gas is logical
Amount is 188m3/(m2·h·kPa)。
Embodiment 4
By silicon carbide:Sintering aid：Active powdered carbon：Methylcellulose is 74 by mass percentage:4:20:2 carry out configuration powder,
Wherein sintering aid is made of neopelex and zirconium oxide, ratio 1:1.The quality of powder, water, glycerol, paraffin
Percentage is 100:11:2:2, the wet feed being stirred is put into vacuum deairing machine and carries out pugging, the number of pugging is 1 time, very
Reciprocal of duty cycle is 0.09 MPa, obtains the preferable mud section of plasticity, then the mud section got is placed in extruder by plasticity index 0.5
In pug cylinder, is squeezed out under the constant pressure of 12 MPa and obtain a length of 1500mm, outer diameter 60mm, the green compact of internal diameter 40mm.Green compact are placed
It is dried in customized V-groove, drying procedure is 4 h at 40 DEG C, 24 h at 80 DEG C.The liter that sintering procedure is 0 ~ 500 DEG C
Warm rate is 0.5 DEG C/min, and 500 DEG C of 2 h of heat preservation, 500 ~ 1000 DEG C of heating rates are 10 DEG C/min, 1000 ~ 1150 DEG C of heating
Rate is 1 DEG C/min, and Temperature fall after 2h is kept the temperature at 1150 DEG C.
The performance of gained supporter is as follows, and aperture is 32 μm, porosity 45%, and breaking load is 3401 N, air flux
For 90 m3/(m2·h·kPa)。
Embodiment 5
By silicon carbide:Sintering aid：Active powdered carbon：Methylcellulose is 74 by mass percentage:4:20:2 carry out configuration powder,
Wherein sintering aid is made of neopelex and zirconium oxide, ratio 1:1.The quality of powder, water, glycerol, paraffin
Percentage is 100:12:2:2, the wet feed being stirred is put into vacuum deairing machine and carries out pugging, the number of pugging is 6 times, very
Reciprocal of duty cycle is 0.08 MPa, obtains the preferable mud section of plasticity, then the mud section got is placed in extruder by plasticity index 0.3
It in pug cylinder, is squeezed out under the constant pressure of 10 MPa and obtains 34.6 mm of outer diameter, the green compact in 19 channels, length can be according to requiring to intercept.
Green compact are placed in customized V-groove and are dried, and drying procedure is 4 h at 40 DEG C, 24 h at 80 DEG C.Sintering procedure be 0 ~
500 DEG C of heating rate is 0.5 DEG C/min, 500 DEG C of heat preservation 2 h, and 500 ~ 1000 DEG C of heating rates are 10 DEG C/min, 1000 ~
1150 DEG C of heating rate is 1 DEG C/min, and Temperature fall after 4 h is kept the temperature at 1150 DEG C.
The performance of gained supporter is as follows, 31 μm of aperture, porosity 45.3%, and breaking load is 3190 N.
Comparative example 1
For the present embodiment the difference from embodiment 1 is that plasticizer glycerol is not added, remaining step is same as Example 1.
Mixed powder is placed in blender, the mass percent of powder and liquid is powder：Water：Paraffin=100:
10:5, after liquid is added several times, carry out that 2 h are sufficiently stirred.The wet feed being stirred is put into vacuum deairing machine and carries out pugging,
The number of pugging is 4 ~ 6 times, and vacuum degree is 0.08 ~ 0.09 MPa.Then mud section is placed in the pug cylinder of extruder, 8
It carries out squeezing out outer diameter under the constant pressure of MPa being 40 mm, internal diameter is the green compact of 30 mm, and length can be according to requiring to intercept.Green compact are put
It sets and is dried in customized V-groove, drying procedure is 4 h at 40 DEG C, 12 h at 80 DEG C.The green body being baked is put into high temperature
It is sintered in electric furnace, 0 ~ 500 DEG C of heating rate is 2 DEG C/min, and 500 DEG C of 2 h of heat preservation, 500 ~ 1000 DEG C of heating rates are 10
DEG C/min, 1000 ~ 1150 DEG C of heating rate is 1 DEG C/min, and Temperature fall after 2 h is kept the temperature at 1150 DEG C.
Comparative example 2
The present embodiment is the difference from embodiment 1 is that pugging number, remaining step are same as Example 1.
Mixed powder is placed in blender, the mass percent of powder and liquid is powder：Water：Paraffin：Glycerol=
100:10:5, after liquid is added several times, carry out that 2 h are sufficiently stirred.The wet feed being stirred is put into vacuum deairing machine and is carried out
Pugging, the number of pugging are 1 time, and vacuum degree is 0.08 ~ 0.09 MPa.Then mud section is placed in the pug cylinder of extruder,
It carries out squeezing out outer diameter under the constant pressure of 8MPa being 40 mm, internal diameter is the green compact of 30 mm, and length can be according to requiring to intercept.Green compact are put
It sets and is dried in customized V-groove, drying procedure is 4 h at 40 DEG C, 12 h at 80 DEG C.The green body being baked is put into high temperature
It is sintered in electric furnace, 0 ~ 500 DEG C of heating rate is 2 DEG C/min, and 500 DEG C of 2 h of heat preservation, 500 ~ 1000 DEG C of heating rates are 10
DEG C/min, 1000 ~ 1150 DEG C of heating rate is 1 DEG C/min, and Temperature fall after 2h is kept the temperature at 1150 DEG C.
Comparative example 3
For the present embodiment the difference from embodiment 1 is that the vacuum degree of pugging is different, remaining step is same as Example 1.
Mixed powder is placed in blender, the mass percent of powder and liquid is powder：Water：Paraffin=100:
10:5, after liquid is added several times, carry out that 2 h are sufficiently stirred.The wet feed being stirred is put into vacuum deairing machine and carries out pugging,
The number of pugging is 4 ~ 6 times, vacuum degree 0.05MPa.Then mud section is placed in the pug cylinder of extruder, in the perseverance of 8 MPa
Pressure carries out squeezing out outer diameter being 40 mm, and internal diameter is the green compact of 30 mm, and length can be according to requiring to intercept.Green compact are placed on customized
V-groove in dried, drying procedure is 4 h at 40 DEG C, 12 h at 80 DEG C.By the green body being baked be put into high-temperature electric resistance furnace into
Row sintering, 0 ~ 500 DEG C of heating rate are 2 DEG C/min, and 500 DEG C of 2 h of heat preservation, 500 ~ 1000 DEG C of heating rates are 10 DEG C/min,
1000 ~ 1150 DEG C of heating rate is 1 DEG C/min, and Temperature fall after 2 h is kept the temperature at 1150 DEG C.
Comparative example 4
For the present embodiment the difference from embodiment 1 is that sintering temperature is different, remaining step is same as Example 1.
Mixed powder is placed in blender, the mass percent of powder and liquid is powder：Water：Paraffin=100:
10:5, after liquid is added several times, carry out that 2 h are sufficiently stirred.The wet feed being stirred is put into vacuum deairing machine and carries out pugging,
The number of pugging is 4 ~ 6 times, and vacuum degree is 0.05 MPa.Then mud section is placed in the pug cylinder of extruder, in the perseverance of 8 MPa
Pressure carries out squeezing out outer diameter being 40 mm, and internal diameter is the green compact of 30 mm, and length can be according to requiring to intercept.Green compact are placed on customized
V-groove in dried, drying procedure is 4 h at 40 DEG C, 12 h at 80 DEG C.By the green body being baked be put into high-temperature electric resistance furnace into
Row sintering, 0 ~ 500 DEG C of heating rate are 2 DEG C/min, and 500 DEG C of 2 h of heat preservation, 500 ~ 1000 DEG C of heating rates are 10 DEG C/min,
1000 ~ 1050 DEG C of heating rate is 1 DEG C/min, and Temperature fall after 2 h is kept the temperature at 1050 DEG C.
31 μm of the following aperture of the performance of gained supporter, porosity 47.2%, breaking load is 891 N, and is lost powder
The phenomenon that, 131 m of air flux3/(m2·h·kPa)。
The performance of 1 silicon carbide supporter of table
Claims (6)
1. a kind of method of extrusion molding low-temperature preparation of porous silicon carbide ceramic, which is characterized in that
（1）By silicon carbide, pore creating material, sintering aid, binder, which is placed in by a certain percentage in three-dimensional material mixer, mixes 12 ~ 24 h,
40 ~ 60 r/min of revolving speed；
（2）Plasticizer, lubricant, water are added in powder upon mixing, is stirred in high-speed mixer by a certain percentage
0.5 ~ 1h, 240 ~ 360 r/min of mixing speed；
（3）By wet feed made from step 2, vacuum pugging is carried out, the preferable mud column of plasticity is obtained；
（4）The mud column of different plasticity made from step 3 is placed in extruder and carries out extrusion molding；
（5）The green compact that step 4 is obtained be put into baking oven according to different wall thickness be arranged distinct program dried, de-waxing, then into
Row sintering.
2. the method that extrusion molding according to claim 1 prepares porous silicon carbide ceramic pipe, which is characterized in that step
（1）The silicon carbide average grain diameter is 100 ~ 200 μm, and sintering aid selects zirconium oxide and neopelex, pore-creating
Agent is active powdered carbon, and partial size is 5 ~ 20 μm, and binder is methylcellulose, and the mass percent of each component is silicon carbide：Sintering
Auxiliary agent：Pore creating material：Binder=71 ~ 76：2~7：20：2.
3. the method that extrusion molding according to claim 1 prepares porous silicon carbide ceramic pipe, which is characterized in that step
（2）The plasticizer is glycerol, and lubricant is paraffin；The mass percent of each substance is powder：Water：Glycerol：Paraffin=100:
10~12：1~5：1~5.
4. the method that extrusion molding according to claim 1 prepares porous silicon carbide ceramic pipe, which is characterized in that step
（3）Pugging condition is 0.08 ~ 0.09 MPa of vacuum degree, and pugging number 1 ~ 6 time, the mud column practised is without obvious crackle.
5. the method that extrusion molding according to claim 1 prepares porous silicon carbide ceramic pipe, which is characterized in that step
（4）The extrusion condition of the different plasticity index mud column is 6 ~ 12 MPa.
6. the method that extrusion molding according to claim 1 prepares porous silicon carbide ceramic pipe, which is characterized in that step
（5）The drying procedure is, after drying 4 h in baking oven at 40 DEG C, then 12 ~ 24 h is dried at 80 DEG C；The sintering
Program is, 0 ~ 500 DEG C of heating rate is 0.5 ~ 2 DEG C/min, 500 DEG C of 2 h of heat preservation, 500 ~ 1000 DEG C of heating rates for 10 DEG C/
Min, 1000 ~ 1150 DEG C of heating rate are 1 DEG C/min, and Temperature fall after 2 ~ 3 h is kept the temperature at 1150 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811048791.XA CN108911779A (en) | 2018-09-10 | 2018-09-10 | Method for preparing porous silicon carbide ceramic tube at low temperature through extrusion molding |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811048791.XA CN108911779A (en) | 2018-09-10 | 2018-09-10 | Method for preparing porous silicon carbide ceramic tube at low temperature through extrusion molding |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108911779A true CN108911779A (en) | 2018-11-30 |
Family
ID=64408147
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811048791.XA Pending CN108911779A (en) | 2018-09-10 | 2018-09-10 | Method for preparing porous silicon carbide ceramic tube at low temperature through extrusion molding |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108911779A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124526A (en) * | 2019-04-30 | 2019-08-16 | 湖北工业大学 | A kind of production method of silicon carbide inorganic ceramic membrane |
| CN110743282A (en) * | 2019-11-07 | 2020-02-04 | 南京工业大学 | Reducing gas purification ceramic filtration membrane tube |
| CN112692966A (en) * | 2020-12-29 | 2021-04-23 | 北方民族大学 | Thin-wall silicon carbide pipe anti-deformation extrusion molding process and special anti-deformation support |
| CN113648848A (en) * | 2021-08-05 | 2021-11-16 | 河北工业大学 | Hollow flat ceramic membrane and preparation method thereof |
| CN114085090A (en) * | 2021-11-22 | 2022-02-25 | 顾江龙 | Honeycomb ceramic combustion plate and sintering method thereof |
| CN115010505A (en) * | 2022-06-01 | 2022-09-06 | 山东百川智能科技有限公司 | Pressureless sintering high thermal shock resistance silicon carbide ceramic heat exchanger tube and processing method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1953855A (en) * | 2004-05-12 | 2007-04-25 | 液体空气乔治洛德方法利用和研究的具有监督和管理委员会的有限公司 | Method for the production of ceramic catalytic membrane reactors by co-extrusion |
| CN101406782A (en) * | 2008-11-06 | 2009-04-15 | 山东理工大学 | Method for producing silicon carbide porous ceramic filtering element and extrusion apparatus |
| CN101642651A (en) * | 2009-08-25 | 2010-02-10 | 山东理工大学 | Preparation method of filter element of fly-ash filter for clean coal power generation |
| CN105461306A (en) * | 2015-11-16 | 2016-04-06 | 石婷 | High-strength silicon carbide ceramic pipe and manufacturing method thereof |
| CN105884394A (en) * | 2016-06-20 | 2016-08-24 | 南京工业大学 | Method for preparing porous silicon carbide support body at low temperature |
-
2018
- 2018-09-10 CN CN201811048791.XA patent/CN108911779A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1953855A (en) * | 2004-05-12 | 2007-04-25 | 液体空气乔治洛德方法利用和研究的具有监督和管理委员会的有限公司 | Method for the production of ceramic catalytic membrane reactors by co-extrusion |
| CN101406782A (en) * | 2008-11-06 | 2009-04-15 | 山东理工大学 | Method for producing silicon carbide porous ceramic filtering element and extrusion apparatus |
| CN101642651A (en) * | 2009-08-25 | 2010-02-10 | 山东理工大学 | Preparation method of filter element of fly-ash filter for clean coal power generation |
| CN105461306A (en) * | 2015-11-16 | 2016-04-06 | 石婷 | High-strength silicon carbide ceramic pipe and manufacturing method thereof |
| CN105884394A (en) * | 2016-06-20 | 2016-08-24 | 南京工业大学 | Method for preparing porous silicon carbide support body at low temperature |
Non-Patent Citations (1)
| Title |
|---|
| 袁林等: "《绿色耐火材料》", 31 January 2015, 中国建材工业出版社 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124526A (en) * | 2019-04-30 | 2019-08-16 | 湖北工业大学 | A kind of production method of silicon carbide inorganic ceramic membrane |
| CN110743282A (en) * | 2019-11-07 | 2020-02-04 | 南京工业大学 | Reducing gas purification ceramic filtration membrane tube |
| CN110743282B (en) * | 2019-11-07 | 2021-04-20 | 南京工业大学 | Reducing gas purification ceramic filtration membrane tube |
| CN112692966A (en) * | 2020-12-29 | 2021-04-23 | 北方民族大学 | Thin-wall silicon carbide pipe anti-deformation extrusion molding process and special anti-deformation support |
| CN112692966B (en) * | 2020-12-29 | 2022-01-11 | 北方民族大学 | Thin-wall silicon carbide pipe anti-deformation extrusion molding process and special anti-deformation support |
| CN113648848A (en) * | 2021-08-05 | 2021-11-16 | 河北工业大学 | Hollow flat ceramic membrane and preparation method thereof |
| CN113648848B (en) * | 2021-08-05 | 2023-12-08 | 河北工业大学 | Hollow flat ceramic membrane and preparation method thereof |
| CN114085090A (en) * | 2021-11-22 | 2022-02-25 | 顾江龙 | Honeycomb ceramic combustion plate and sintering method thereof |
| CN115010505A (en) * | 2022-06-01 | 2022-09-06 | 山东百川智能科技有限公司 | Pressureless sintering high thermal shock resistance silicon carbide ceramic heat exchanger tube and processing method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108911779A (en) | Method for preparing porous silicon carbide ceramic tube at low temperature through extrusion molding | |
| CN105601279B (en) | The method that injection forming and solid-phase sintering prepare thin-wall construction silicon carbide ceramics | |
| TWI430975B (en) | Composition for ceramic extrusion-molded body and method for manufacturing a ceramic extrusion-molded body | |
| CN111574226B (en) | Preparation method of high-density low-free silicon content reaction sintered silicon carbide ceramic material | |
| CN109437959B (en) | Method for preparing mullite fiber-based porous ceramic by using environment-friendly gel casting | |
| CN105175005A (en) | Preparation method of high-strength uniform-hole silicon carbide ceramic membrane | |
| CN106565226B (en) | A kind of tape casting preparation of the alumina silicate porous ceramic film material with three-dimensional net structure | |
| CN104944930B (en) | A kind of fire resistant sagger and preparation method thereof | |
| CN105016751B (en) | A kind of method that utilization grain composition attached gel molding process prepares aircon refractory | |
| CN111004018B (en) | High-temperature phase-change heat storage material, heat storage brick and preparation method thereof | |
| CN113999046B (en) | Preparation method of low-temperature reaction sintered silicon carbide ceramic membrane | |
| CN106380201A (en) | Method for preparing specially-shaped boron carbide ceramics | |
| CN106336197B (en) | Electron ceramic material is fired with saggar and preparation method thereof | |
| CN106268334B (en) | A kind of ceramic separation film element and preparation method thereof | |
| CN105439620A (en) | Method for preparing porous silicon nitride by spark plasma sintering | |
| CN108395232B (en) | Preparation method of cordierite-based porous ceramic with high seepage rate | |
| CN106007779B (en) | The preparation method of high purity aluminium oxide flat ceramic film support | |
| CN102718510B (en) | Non-burning permeable brick for steel ladle bottom argon bubbling and preparation process thereof | |
| CN107814583A (en) | A kind of Al4O4Silicon carbide honeycomb ceramics of C enhancings and preparation method thereof | |
| CN102335950A (en) | Forming method of ceramic biscuit with impact resisting structure | |
| CN101636365A (en) | Additives comprising cellulose ethers for ceramics extrusion | |
| CN103274692A (en) | Unfired SiC kiln furniture material and production method thereof | |
| CN111393156A (en) | Preparation method of cordierite porous ceramic | |
| CN110950664A (en) | Light high-strength silicon carbide energy-saving kiln furniture and preparation method thereof | |
| CN109516831A (en) | A kind of preparation method of aluminum oxide porous material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20201111 Address after: 211800 Jiangsu Nanjing Pukou District Qiaolin street Pukou Economic Development Zone No. 29 Applicant after: Jiangsu Jiulang High-Tech Co.,Ltd. Applicant after: Nanjing Tech University Address before: 211800, Pukou District, Jiangsu City, Nanjing Province Park No. 1 Applicant before: NANJING MEMBRANE MATERIALS INDUSTRY TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. Applicant before: Nanjing Tech University |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181130 |