CN114524675A - Silicon-bonded silicon carbide diesel particulate filter and preparation method thereof - Google Patents
Silicon-bonded silicon carbide diesel particulate filter and preparation method thereof Download PDFInfo
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- CN114524675A CN114524675A CN202210162264.1A CN202210162264A CN114524675A CN 114524675 A CN114524675 A CN 114524675A CN 202210162264 A CN202210162264 A CN 202210162264A CN 114524675 A CN114524675 A CN 114524675A
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- silicon carbide
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- diesel particulate
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 84
- 238000000034 method Methods 0.000 claims abstract description 39
- 238000005238 degreasing Methods 0.000 claims abstract description 25
- 230000001681 protective effect Effects 0.000 claims abstract description 23
- 239000012298 atmosphere Substances 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 22
- 238000005520 cutting process Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 238000001125 extrusion Methods 0.000 claims abstract description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 claims abstract description 3
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 239000011230 binding agent Substances 0.000 claims description 42
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 31
- 229910052751 metal Inorganic materials 0.000 claims description 26
- 239000002184 metal Substances 0.000 claims description 26
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
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- 125000003158 alcohol group Chemical group 0.000 claims description 2
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052710 silicon Inorganic materials 0.000 description 24
- 239000010703 silicon Substances 0.000 description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 19
- 230000000694 effects Effects 0.000 description 17
- 229910052681 coesite Inorganic materials 0.000 description 16
- 229910052906 cristobalite Inorganic materials 0.000 description 16
- 239000000377 silicon dioxide Substances 0.000 description 16
- 229910052682 stishovite Inorganic materials 0.000 description 16
- 229910052905 tridymite Inorganic materials 0.000 description 16
- 239000000919 ceramic Substances 0.000 description 15
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- 238000009826 distribution Methods 0.000 description 12
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- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 12
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- 150000003077 polyols Chemical class 0.000 description 11
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 230000001965 increasing effect Effects 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 230000000903 blocking effect Effects 0.000 description 6
- 229910052878 cordierite Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 5
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- 238000007580 dry-mixing Methods 0.000 description 2
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- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
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- 229910052914 metal silicate Inorganic materials 0.000 description 1
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- 231100000719 pollutant Toxicity 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
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- 229910021493 α-cristobalite Inorganic materials 0.000 description 1
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Abstract
The invention belongs to the technical field of diesel particulate filters, and particularly relates to a silicon-bonded silicon carbide diesel particulate filter and a preparation method thereof. The method comprises the following steps: 1) selecting required raw materials, preparing the raw materials into mud segments, performing extrusion forming to obtain green bodies, performing microwave drying, and cutting and forming the dried green bodies into single square substrates; 2) carrying out a plugging process on the single square substrate to form a green body; 3) sequentially carrying out fine degreasing sintering, protective atmosphere sintering and oxidizing sintering on the green body to obtain a cooked blank; 4) the cooked blank is spliced into a cuboid shape in a bonding mode and is subjected to post-treatment to obtain the finished product. The invention solves the problems of difficult sintering, high manufacturing cost, easy cracking and poor micropore connectivity of the existing silicon carbide diesel particle filter, and obviously reduces the production cost of the silicon carbide diesel particle filter.
Description
Technical Field
The invention belongs to the technical field of diesel particulate filters, and particularly relates to a silicon-bonded silicon carbide diesel particulate filter and a preparation method thereof.
Background
With the increasingly strict requirements on the domestic automobile exhaust emission and the increasing demand on the diesel particulate filter, the mainstream catalyst carrier materials in the market mainly comprise cordierite, silicon carbide, aluminum titanate, acicular mullite and the like. Wherein, the filter made of acicular mullite has the characteristics of high CTE and easy generation of pollutants such as chloride, fluoride and the like, and the sale market is not wide; the filter made of the aluminum titanate material has the defects of low mechanical strength, fragile packaging, and easy decomposition into titanium dioxide, which causes the rapid increase of the thermal expansion coefficient of the product and the generation of cracks. The current market acceptance is higher for diesel vehicle filters made of cordierite and silicon carbide. For the traditional cordierite porous ceramics, the price is low, but the highest temperature resistance is generally not more than 1300 ℃, the use temperature is low, and the cordierite porous ceramics are easy to damage and have poor corrosion resistance, thereby causing disastrous accidents. Although the high-temperature strength of the porous ceramic made of silicon carbide can be maintained to be more than 1600 ℃, different technical routes are provided for preparing the diesel particle filter made of silicon carbide in China, and each method has the advantages and disadvantages of the method, for example, the recrystallized silicon carbide has the characteristics of narrow pore size distribution and low CTE, but the sintering temperature of the recrystallized silicon carbide exceeds 2300 ℃, the manufacturing cost is high, the sintering is difficult, and products made of other oxides or cordierite combined with silicon carbide have the disadvantages of poor pore connectivity, easy cracking, difficult control of the CTE and extremely high use risk.
Therefore, in order to meet the market demand, the development of a diesel particulate filter which has low cost, narrow pore diameter distribution, good pore connectivity, difficult cracking and high temperature resistance strength is urgent. The technological method adopts metal silicon with CTE and thermal conductivity close to those of silicon carbide material as a binder, and sintering aids such as silica sol or alumina sol are added to the binder to form a mixture containing CH4Or Ar or H2Or CO2Sintering in a micro-positive pressure mode under the sintering of the protective atmosphere, and forming SiO on the surface of the product through advanced oxidation treatment2The oxidation resistant film ensures that the product has high oxidation resistance, has the advantages of retaining the advantages of excellent mechanical property, high temperature resistance strength, good oxidation resistance and the like of the silicon carbide material, and strictly controls the formation of SiO by degreasing sintering, micro-positive pressure sintering in protective atmosphere and oxidation pretreatment sintering2The position and content of the compound ensure that the CTE performance of the product is excellent. Compared with recrystallized silicon carbide material, the sintering cost of the silicon carbide porous ceramic is greatly reduced, compared with other substance-bonded silicon carbide materials, the stability and the pore connectivity of the CTE of the product are strictly controlled, the high temperature resistance strength of the product and the use durability of the silicon-bonded silicon carbide porous ceramic are ensured, the metal silicon glass phase has a certain adhesive effect, the compressive strength of the porous ceramic is greatly improved, and the SiO formed on the surface of the metal silicon glass phase2The film also greatly improves the oxidation resistance of the product. In the sintering process, micropores with good connectivity can be formed by melting and wrapping the metal silicate glass phase, so that the filtering efficiency is improved, and excellent pore distribution is obtained. The added sintering aid has a certain wetting effect on the melting process of the metal silicon, ensures the uniformity of melting and wrapping of the metal silicon and further ensures the uniform and narrow distribution of micropores of the product. In the aspect of raw material selection, the technology adopts shaped silicon carbide particles with narrow particle size distributionAnd the powder is prepared from a metal silicon raw material with narrow particle size distribution, so that the consistency of the sintering process is ensured, the formed micropores are narrow in distribution, good in connectivity and appropriate in particle micro-morphology.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a silicon-bonded silicon carbide diesel particulate filter and a preparation method thereof. The invention solves the problems of difficult sintering, high manufacturing cost, easy cracking and poor micropore connectivity of the existing silicon carbide diesel particle filter, obviously reduces the production cost of the silicon carbide diesel particle filter, simultaneously adds one or two of silica sol or aluminum sol, achieves the effects of enhancing the strength of a degreasing sintering semi-finished product and uniformly coating molten metal, and improves the production efficiency and the product percent of pass. The silicon-bonded silicon carbide diesel particulate filter has the advantages of low cost, high temperature resistance, good oxidation resistance, narrow pore diameter distribution and good pore connectivity.
The technical scheme provided by the invention is as follows:
a method of making a silicon-bonded silicon carbide diesel particulate filter, comprising the steps of:
1) selecting required raw materials, preparing the raw materials into mud segments, performing extrusion forming to obtain green bodies, performing microwave drying, and cutting and forming the dried green bodies into single square substrates;
2) carrying out a plugging process on the single square substrate obtained in the step 1) to form a green body with a cross hole on one side and a hole on one end of a single pore passage and a hole on the other end for plugging;
3) sequentially carrying out fine degreasing sintering, protective atmosphere sintering and oxidizing sintering on the green body obtained in the step 2) to obtain a cooked blank with high strength and narrow pore size distribution;
4) the cooked blank is spliced into a cuboid shape with required specification and shape by a bonding mode, and is subjected to post-treatment to manufacture the silicon-bonded silicon carbide-based diesel particle filter, which can be called as silicon-bonded silicon carbide-based porous ceramic;
wherein, the raw materials comprise inorganic main materials and additives;
the inorganic main material comprises the following components in percentage by mass based on the total weight of the inorganic main material:
65-85 wt% of silicon carbide micro powder;
15-35 wt% of metal silicon powder;
the additive comprises the following components in percentage by mass based on the total amount of the inorganic main materials:
0-40 wt% of pore-forming agent;
6-10 wt% of organic binder.
In the prior art, a silicon carbide diesel particulate filter is generally sintered at a high temperature under a protective atmosphere, but the sintering mode has the problems of high cost and low production efficiency caused by complicated working procedures. According to the technical scheme, the novel adhesive is used for combining the silicon carbide particles, so that the manufacturing cost is low, the temperature resistance is high, the oxidation resistance is good, and the problems of high cost and low production efficiency are fundamentally solved. Specifically, the following effects are exhibited:
the electrical conductivity of the metal silicon has a great relationship with the temperature thereof, the electrical conductivity increases with the temperature rise and reaches the maximum at about 1480 ℃, the temperature decreases with the temperature rise after exceeding 1600 ℃, the matching degree with the thermal expansion coefficient and the thermal conductivity of the silicon carbide material is very high, the thermal conductivity of the product in the use process is close to that of the silicon carbide, and the risk of product cracking caused by inconsistent thermal conductivity of the product is reduced.
Meanwhile, the metal silicon glass phase also has a certain gluing effect, is melted and wrapped around the silicon carbide particles, and has excellent oxidation resistance and normal-temperature mechanical properties.
And, SiO formed by pre-oxidation treatment2The protective film has excellent thermal stability and oxidation resistance, and the excellent performance is derived from SiO2Compactness of oxide film and SiO2Stability of crystal form, and SiO2The basic structural units of the crystal structure are all silicon-oxygen tetrahedrons, SiO2During the oxidation pretreatment sintering process, the crystal forms gradually form quartz crystal phases with thermal stability over 1600 ℃, such as alpha-cristobalite or quartz glass, and the like, so that the crystal forms have higher matching degree with the melting point of silicon carbide, and the porous silicon carbide-silicon combined metal is ensuredThe ceramic has excellent temperature resistance. The diesel particle filter made of the material is completely sintered in a micro-positive pressure protective atmosphere at about 1600 ℃, so that the excellent CTE (coefficient of thermal expansion) performance of the product is ensured, and the risk of cracking of the product in the use process is reduced.
The protective atmosphere used therein is mainly one or more of reducing or inert gases, such as: ar, CH4、H2、CO、CO2And the like. The amount of pore-forming agent is not zero.
In step 1), a mud segment is prepared on the basis of the kneading step. The weight percentage of water added in the kneading step to the total powder is 15 to 22 wt%.
Further, the raw materials also comprise the following components in percentage by mass based on the total amount of the inorganic main materials and the additives:
0.5-3 wt% of dispersant;
0.5-3 wt% of lubricant;
1-10 wt% of sintering aid.
Specifically, the method comprises the following steps:
the pore-forming agent is one or more of starch, resin, carbon powder or fiber.
The organic binder is alcohols and/or celluloses;
the dispersing agent is alcohol ether;
the lubricant is oil;
the sintering aid is silicon-aluminum sol.
The raw materials adopted by the invention can be selected from the materials in the prior art.
Specifically, in the step 1), the bottom surface of the obtained single square base body is square, and the side length of the single square base body is 1.5-2 inches.
Specifically, the post-treatment in the step 1) comprises the steps of edging, end face smoothing, seam beautifying, edge surrounding, burning back and the like.
The invention also provides the silicon-bonded silicon carbide diesel particulate filter prepared by the preparation method.
Drawings
FIG. 1 is an SEM image of shaped silicon carbide powder used in the present invention;
FIG. 2 is an SEM image of shaped silicon metal powder used in the present invention;
FIG. 3 is an SEM micrograph of a silicon-bonded silicon carbide-based porous ceramic provided by the present invention;
FIG. 4 is an SEM micrograph of a silicon-bonded silicon carbide-based porous ceramic provided by the present invention;
FIG. 5 is a main process flow of the silicon-bonded silicon carbide-based porous ceramic provided by the present invention;
FIG. 6 is a distribution diagram of micropores of a silicon-bonded silicon carbide-based porous ceramic provided by the present invention;
FIG. 7 is a schematic representation of a silicon-bonded silicon carbide diesel particulate filter product provided by the present invention.
Detailed Description
The principles and features of the present invention are described below, and the examples are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
(1) Dry mixing 75 wt% of 25-28 micron silicon carbide powder and 25 wt% of 3-6 micron metal silicon. The inorganic main material is taken as 100 percent of total weight, 3 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added to prepare a uniform mixture with close packing. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 22 wt% of water of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, and kneading for 25 minutes, wherein the additive is added based on the total mixed components, in order to increase the plasticity, lubricity and surface activity of the pug, organic additives such as soybean oil, butter, surfactant and the like can be adopted, and butter and polyether polyol with equal mass ratio are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) the invention extrudes the mud segment with plasticity into a honeycomb structure, and extrudes raw mud with the outer skin of 40X 189mmCarrying out microwave and drying on the blank; (5) cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole blocking process, wherein the depth of a plug is 8-10mm, and processing the square small holes of the product into holes with one end blocked and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Example 2
(1) 75 percent of silicon carbide micro powder with the weight of 25-28 mu m and 25 percent of metal silicon with the weight of 3-6 mu m are mixed by a dry method. Taking the total weight of the inorganic main materials as 100 percent, adding 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder by weight to prepare a uniform mixture with close packing. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 22 wt% of water of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, and kneading for 25 minutes, wherein the additive is added based on the total mixed components, in order to increase the plasticity, lubricity and surface activity of the pug, organic additives such as soybean oil, butter, surfactant and the like can be adopted, and butter and polyether polyol with equal mass ratio are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with an outer skin of 40X 189mm, and then carrying out microwave drying; (5) and cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole plugging process, wherein the plug depth is 8-10mm, and processing the square small holes of the product into holes with one end plugged and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. In a vacuum which can be filled with inert gasSintering in protective atmosphere at 1450 deg.c, and melting and wrapping silicon metal around the silicon carbide grains to form high adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Example 3
(1) 75 percent of silicon carbide micro powder with the weight of 25-28 mu m and 25 percent of metal silicon with the weight of 3-6 mu m are mixed by a dry method. The inorganic main material is taken as 100 percent of total weight, 10 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 22 wt% of water of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, and kneading for 25 minutes, wherein the additive is added on the basis of the total mixed components, and in order to increase the plasticity, lubricity and surface activity of the pug, organic additives such as soybean oil, butter, surfactant and the like can be adopted, and butter and polyether polyol are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) and cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole plugging process, wherein the plug depth is 8-10mm, and processing the square small holes of the product into holes with one end plugged and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Example 4
(1) Mixing 70% of 25-28 μm silicon carbide micropowder 30% by weight by a dry methodMetallic silicon with a weight of 3-6 μm. The inorganic main material is taken as 100 percent of total weight, 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 22 wt% of water of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, and kneading for 25 minutes, wherein the additive is added on the basis of the total mixed components, and in order to increase the plasticity, lubricity and surface activity of the pug, organic additives such as soybean oil, butter, surfactant and the like can be adopted, and butter and polyether polyol are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and cutting the pug sections into sections after 3 times of slicing; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole blocking process, wherein the depth of a plug is 8-10mm, and processing the square small holes of the product into holes with one end blocked and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Example 5
(1) 75 percent of silicon carbide micro powder with the weight of 25-28 mu m and 25 percent of metal silicon with the weight of 3-6 mu m are mixed by a dry method. The inorganic main material is taken as 100 percent of total weight, 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) mixing the mixed powderPlacing the mixture in a kneading machine, adding 22 wt% of water of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, and kneading for 25 minutes, wherein the additive is added based on the total mixed components, and in order to increase the plasticity, lubricity and surface activity of the pug, organic additives such as soybean oil, butter, surfactant and the like can be adopted, and butter and polyether polyol are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole blocking process, wherein the depth of a plug is 8-10mm, and processing the square small holes of the product into holes with one end blocked and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Example 6
(1) 80 percent of silicon carbide micro powder with the particle size of 25-28 mu m and 20 percent of metal silicon with the particle size of 3-6 mu m are mixed by a dry method. The inorganic main material is taken as 100 percent of total weight, 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) the mixed powder is put into a kneading machine and added with 22 wt% of water of the total powder for kneading for 17 minutes, 1.0 wt% of lubricant and 1 wt% of dispersant are added for kneading for 25 minutes, the additive is added on the basis of the total mixed components, in order to increase the plasticity, lubricity and surface activity of the pug, organic additives such as soybean oil, butter, surfactant and the like can be adopted, and butter and polyether multi-component are adopted in the embodimentAn alcohol; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole blocking process, wherein the depth of a plug is 8-10mm, and processing the square small holes of the product into holes with one end blocked and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Example 7
(1) 75 percent of silicon carbide micro powder with the weight of 25-28 mu m and 25 percent of metal silicon with the weight of 3-6 mu m are mixed by a dry method. The inorganic main material is taken as 100 percent of total weight, 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 15 wt% of water and 7 wt% of acid silica sol of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, kneading for 25 minutes, wherein the additive is added based on the total mixed components, and organic additives such as soybean oil, butter, surfactant and the like can be adopted for the purpose of increasing the plasticity, lubricity and surface activity of the pug, and butter and polyether polyol are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and cutting the pug sections into sections after 3 times of slicing; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) cutting the dried green body into pieces with fixed height of 177.8mm, performing laser drilling-hole blocking process with the depth of 8-10mm, and making the square small holes on the productOne end is blocked and the other end is provided with a hole. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Example 8
(1) 75 percent of silicon carbide micro powder with the weight of 25-28 mu m and 25 percent of metal silicon with the weight of 3-6 mu m are mixed by a dry method. The inorganic main material is taken as 100 percent of total weight, 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 15 wt% of water and 7 wt% of acid alumina sol of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, kneading for 25 minutes, wherein the additive is added based on the total mixed components, and organic additives such as soybean oil, butter, surfactant and the like can be adopted for the purpose of increasing the plasticity, lubricity and surface activity of the pug, and butter and polyether polyol are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) and cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole plugging process, wherein the plug depth is 8-10mm, and processing the square small holes of the product into holes with one end plugged and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, about 13 deg.COxidizing and pre-treating at 50 deg.c to sinter to form compact SiO2And (5) protecting the film.
Example 9
(1) 75 percent of silicon carbide micro powder with the weight of 25-28 mu m and 25 percent of metal silicon with the weight of 3-6 mu m are mixed by a dry method. The inorganic main material is taken as 100 percent of total weight, 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 15 wt% of water and 3 wt% of acidic silica sol and 4 wt% of acidic aluminum sol of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, kneading for 25 minutes, wherein the additive is added on the basis of the total mixed components, and organic additives such as soybean oil, butter, surfactant and the like can be adopted for increasing the plasticity, lubricity and surface activity of the pug, and butter and polyether polyol are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) and cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole plugging process, wherein the plug depth is 8-10mm, and processing the square small holes of the product into holes with one end plugged and the other end perforated. (6) Sintering the green product: a, degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Comparative example 1
(1) 75 percent of silicon carbide micro powder with the weight of 25-28 mu m and 25 percent of metal silicon with the weight of 3-6 mu m are mixed by a dry method. Taking the total weight of the inorganic main materials as 100 percent, and adding 5 percent of starch with the weight of 20-25 mu m9% by weight of organic binder, a homogeneous mixture with close packing was obtained. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET, silica sol, aluminum sol and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 19 wt% of water and 3 wt% of acid silica sol of the total powder, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, kneading for 25 minutes, wherein the additive is added based on the total mixed components, and organic additives such as soybean oil, butter, surfactant and the like can be adopted for the purpose of increasing the plasticity, lubricity and surface activity of the pug, and butter and polyether polyol are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) and cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole plugging process, wherein the plug depth is 8-10mm, and processing the square small holes of the product into holes with one end plugged and the other end perforated. (6) Sintering the green product: a, degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Comparative example 2
(1) 75 percent of silicon carbide micro powder with the weight of 25-28 mu m and 25 percent of metal silicon with the weight of 3-6 mu m are mixed by a dry method. The inorganic main material is taken as 100 percent of total weight, 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 19 percent of the total powderKneading water and 3 wt% of acidic aluminum sol for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, and kneading for 25 minutes, wherein the additive is added based on the total mixed components, and organic additives such as soybean oil, butter, and surfactant can be used to increase the plasticity, lubricity, and surface activity of the pug, and butter and polyether polyol are used in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and slicing the pug sections for 3 times to form sections; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) and cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole plugging process, wherein the plug depth is 8-10mm, and processing the square small holes of the product into holes with one end plugged and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
Comparative example 3
(1) Dry mixing 75 wt% of 25-28 micron silicon carbide powder and 25 wt% of 3-6 micron metal silicon. The inorganic main material is taken as 100 percent of total weight, 5 percent of starch with the weight of 20-25 mu m and 9 percent of organic binder are added, and a uniform mixture with close packing is prepared. The addition amounts of the binder and the pore-forming agent are added on the basis of inorganic components, the binder can be selected from methylcellulose, PVA, PET and the like, and hydroxypropyl methylcellulose is adopted in the embodiment; (2) placing the mixed powder into a kneading machine, adding 20 wt% of water and 1 wt% of sintering aid (equal weight ratio of silica sol and aluminum sol) into the kneading machine, kneading for 17 minutes, adding 1.0 wt% of lubricant and 1 wt% of dispersant, kneading for 25 minutes, adding additive based on the total mixed components to increase plasticity, lubricity and surface activity of the pug, and optionally adding soybean oil, butter, surfactant, etcThe organic additive, butter and polyether polyol are adopted in the embodiment; (3) refining the pug kneaded in the step (2) into pug sections, and cutting the pug sections into sections after 3 times of slicing; (4) extruding a mud segment with plasticity into a honeycomb structure, extruding a green body with the outer skin of 40 × 189mm, and then carrying out microwave drying; (5) cutting the dried blank into pieces with fixed height of 177.8mm, performing a laser drilling-hole blocking process, wherein the depth of a plug is 8-10mm, and processing the square small holes of the product into holes with one end blocked and the other end perforated. (6) Sintering the green product: A. degreasing and sintering in an oxidation furnace at about 500 ℃ to remove organic matters of the product. B. Sintering in vacuum filled with inert gas in protective atmosphere at 1450 deg.c to melt and wrap silicon metal around silicon carbide particles to form high-adhesion strength and qualified product. C. In an oxidation furnace, carrying out oxidation pretreatment sintering at about 1350 ℃ to form compact SiO2And (5) protecting the film.
The test results of the examples and comparative examples of the present invention are shown in table one.
The firing curves of the examples and comparative examples given in the present invention are shown in Table II.
For comparison of pressure drop for the embodiments, samples of 143.8mm diameter, 177.8mm height, 300cpsi cell density, and 9mil wall thickness were prepared, although the diameter, height, cell density, and wall thickness of the material are not limited thereto.
This patent lists some examples to illustrate the invention, and should not be construed as limiting the invention, as many modifications are possible.
It can be seen from comparison of examples 1-3 that the higher the pore-forming agent content in the system, the smaller the change in the expansion coefficient of the fired product, the larger the porosity of the product, and the lower the compressive strength, indicating that the addition of the pore-forming agent has a pore-forming tendency, and significantly increasing the number of micropores in the product.
It can be seen from comparison of examples 4-6 that the higher the content of silicon carbide aggregate in the system, the smaller the change of the expansion coefficient and porosity of the fired product, and the lower the median pore diameter and compressive strength, indicating that the addition of silicon metal produces the effect of bond strength, and significantly improves the compressive performance of the product.
Comparing examples 1-3 and comparative examples 4-6, the porosity of the product can be improved by adding the pore-forming agent, the median pore diameter of the product is controlled by the particle size distribution of the pore-forming agent, the content of the aggregate is improved, and the median pore diameter of the product is reduced, so that the optimal strength and filtering performance of the product can be ensured by adding the pore-forming agent and the aggregate with proper contents. The conclusion of the comparative experiment is that the optimal is the example 5, and on the basis, the degreasing strength of the product is further optimized.
In comparison with examples 7-9, before the silicon metal is melted and coated with the silicon carbide particles, in the degreasing and sintering process, one or both of the added silica sol and the added alumina sol have little influence on the product performance, and the degreasing strength of the product is obviously improved, wherein optimally, the silica-alumina sol is added at the same time to react to generate a mullite phase, so that the strength of the product after degreasing, sintering and protective atmosphere sintering is obviously improved.
Comparing with comparative examples 1-3 and examples 7-9, the decrease of the amount of silica sol or alumina sol sintering aid is tried, the degreasing strength of the product is found to decrease with the decrease of the amount of silica-alumina sol, and the experiment of increasing the degreasing strength by examples 7-9 and comparative examples 1-3 shows that the addition of one or two of silica sol or alumina sol which increases the degreasing strength has no obvious influence on the performance of the product, so that the degreasing and sintering strength of green bodies can be increased by adding the sintering aid, and the sintering yield can be increased.
Therefore, the invention uses a more preferable mode similar to the examples 7-9, and uses silicon carbide particles with proper particle size to prepare the metal silicon combined silicon carbide diesel particulate filter by adding metal silicon, silica sol or aluminum sol, and the metal silicon combined silicon carbide diesel particulate filter has excellent micropore distribution and improves the product yield. Meanwhile, the pore-forming agent is added to control the change trend of porosity and pore diameter, the stability of the distribution of the micropores of the porous ceramic is improved, the porous ceramic is sintered by using low-temperature protective atmosphere, and the production cost for preparing the silicon carbide porous ceramic is also greatly reduced.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A method for preparing a silicon-bonded silicon carbide-based diesel particulate filter, comprising the steps of:
1) selecting required raw materials, preparing the raw materials into mud segments, performing extrusion forming to obtain green bodies, performing microwave drying, and cutting and forming the dried green bodies into single square substrates;
2) carrying out a plugging process on the single square substrate obtained in the step 1) to form a green body with a cross hole on one side and a hole on one end of a single pore passage and a hole on the other end for plugging;
3) sequentially carrying out fine degreasing sintering, protective atmosphere sintering and oxidizing sintering on the green body obtained in the step 2) to obtain a cooked blank;
4) splicing the mature blank into a cuboid shape with required specification and shape by a bonding mode, and preparing the silicon-bonded silicon carbide diesel particulate filter by post-treatment;
wherein, the raw materials comprise inorganic main materials and additives;
the inorganic main material comprises the following components in percentage by mass based on the total weight of the inorganic main material:
65-85 wt% of silicon carbide micro powder;
15-35 wt% of metal silicon powder;
the additive comprises the following components in percentage by mass based on the total amount of the inorganic main materials:
0-40 wt% of pore-forming agent;
6-10 wt% of organic binder.
2. The method for preparing a silicon-bonded silicon carbide-based diesel particulate filter according to claim 1, wherein the raw materials further comprise the following components in percentage by mass based on the total amount of the inorganic main materials and the additives:
0.5-3 wt% of dispersant;
0.5-3 wt% of lubricant;
1-10 wt% of sintering aid.
3. The method of making a silicon-bonded silicon carbide-based diesel particulate filter of claim 2, wherein:
the pore-forming agent is selected from one or more of starch, resin, carbon powder or fiber;
the organic binder is alcohols and/or celluloses;
the dispersing agent is alcohol ether;
the lubricant is oil;
the sintering aid is silicon-aluminum sol.
4. The method of making a silicon-bonded silicon carbide-based diesel particulate filter of claim 1, wherein: in the step 1), the dimension of the side length of the bottom surface of the obtained single square matrix is 1.5-2 inches.
5. A silicon-bonded silicon carbide-based diesel particulate filter produced by the production method according to any one of claims 1 to 4.
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