CN115925439B - Silicon carbide particle catcher and preparation method thereof - Google Patents
Silicon carbide particle catcher and preparation method thereof Download PDFInfo
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- CN115925439B CN115925439B CN202211556222.2A CN202211556222A CN115925439B CN 115925439 B CN115925439 B CN 115925439B CN 202211556222 A CN202211556222 A CN 202211556222A CN 115925439 B CN115925439 B CN 115925439B
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 45
- 239000002245 particle Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 11
- 239000005388 borosilicate glass Substances 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000004014 plasticizer Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 74
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 20
- 229910052712 strontium Inorganic materials 0.000 claims description 12
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 12
- 238000007493 shaping process Methods 0.000 claims description 9
- 229920002261 Corn starch Polymers 0.000 claims description 7
- 239000008120 corn starch Substances 0.000 claims description 7
- 235000011187 glycerol Nutrition 0.000 claims description 7
- 229920000609 methyl cellulose Polymers 0.000 claims description 7
- 239000001923 methylcellulose Substances 0.000 claims description 7
- 235000010981 methylcellulose Nutrition 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 239000001856 Ethyl cellulose Substances 0.000 claims description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 2
- 244000017020 Ipomoea batatas Species 0.000 claims description 2
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 235000015895 biscuits Nutrition 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 235000010944 ethyl methyl cellulose Nutrition 0.000 claims description 2
- 229920003087 methylethyl cellulose Polymers 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229920001592 potato starch Polymers 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 229940100445 wheat starch Drugs 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000919 ceramic Substances 0.000 description 11
- 229920003023 plastic Polymers 0.000 description 10
- 238000000034 method Methods 0.000 description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 239000004071 soot Substances 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 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 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention discloses a silicon carbide particle catcher and a preparation method thereof, comprising the following steps: uniformly mixing coarse silicon carbide powder, metal silicon powder and strontium-doped borosilicate glass powder serving as sintering aids, adding pore-forming agents, binders, plasticizers, deionized water and other aids, mixing, pugging, forming, microwave drying, cross hole sealing and high-temperature sintering to finally obtain a silicon carbide particle catcher, and detecting to obtain the silicon carbide with the thermal expansion coefficient of less than or equal to 4.0 x 10 under the condition of 1500 DEG C ‑6 /℃。
Description
Technical Field
The invention relates to a silicon carbide particle catcher and a preparation method thereof.
Background
With the increase of global petroleum resource shortage and CO 2 The pressure of reducing the emission is increased, and the situation of vehicle power diesel engine is foreign. At present, more than 40% of the annual output of European sedans adopts a diesel engine, and the diesel engine is used in France, spanish and other countriesAnd the household time is up to more than 50 percent. Although diesel engines are an environmentally friendly engine as compared to gasoline engines, exhaust emission pollution of diesel vehicles characterized by nitrogen oxides NOx and soot Particulate Matter (PM) becomes an important factor restricting their popularization and application as compared to gasoline vehicles equipped with three-way catalysts. Therefore, development of a diesel soot particulate filter having excellent performance has become a challenge to be solved.
At present, the filter body prepared from the cordierite material still has the defects of low softening temperature and insufficient thermal shock resistance. Silicon carbide is a compound with strong covalent bond, and the ionic type of Si-C bond is only about 12%, so that the silicon carbide has excellent mechanical property, excellent oxidation resistance, high abrasion resistance, low friction coefficient and the like. The silicon carbide ceramic not only has the excellent performance of the porous ceramic, but also has good heat transfer property and thermal stability, however, the filter body combined by silicon carbide and metal oxide also has the problems of high thermal expansion coefficient and insufficient thermal shock resistance, which causes difficult industrial production and application.
Disclosure of Invention
In order to solve the problems of difficult industrial production and application caused by over high thermal expansion coefficient and insufficient shock resistance of a filter body combined with silicon carbide and metal oxide, the invention provides a silicon carbide particle catcher and a preparation method thereof so as to reduce the thermal expansion coefficient of silicon carbide ceramic and adapt to large-scale industrial application, and the specific scheme is as follows:
a method for preparing a silicon carbide particle catcher, comprising the following steps:
s1, preparing a mixture I: mixing coarse silicon carbide powder and metal silicon powder according to a certain proportion to obtain a mixture I;
s2, preparing a mixture II: taking 95-99% of mixture I and 1-5% of sintering aid, and uniformly mixing to obtain mixture II;
s3, preparing a mixture III: adding 2-3% of pore-forming agent, 5-6% of binder, 2-4% of plasticizer and 16-18% of solvent into the mixture II for wet mixing to obtain a mixture III;
s4: putting the mixture III into a vacuum pugging machine for pugging to form a shaping mud blank;
s5: putting the shaped mud blank formed in the step S4 into an extruder, and forming a square honeycomb mud blank unit under the action of a die;
s6: putting the square honeycomb mud blank unit prepared in the step S5 into a microwave drying oven for drying and shaping, and then carrying out cross hole sealing to obtain a silicon carbide blank unit;
s7: putting the monomer biscuit obtained in the step S6 into a high-temperature atmosphere sintering furnace, heating and preserving heat according to a certain sintering curve, and naturally cooling after the heat preservation is finished to obtain a silicon carbide unit;
s8: and (3) bonding the plurality of silicon carbide units obtained in the step (S7) into a whole by using an inorganic bonding material, and drying, excircle processing and skin grafting to obtain the silicon carbide particle catcher.
Further, the weight percentage of the silicon carbide coarse powder and the metal silicon powder in the S1 is 4:1.
further, the heating temperature in S7 is 1300-1700 ℃, and the heat preservation time is 1.5-3 h.
Further, the sintering aid in S2 is strontium-doped borosilicate glass powder, wherein the content of strontium is 5-10%.
Further, the pore-forming agent is one or a mixture of more of corn starch, wheat starch and sweet potato starch.
Further, the binder is one or a mixture of two of methyl cellulose and ethyl cellulose.
Further, the plasticizer is one or a mixture of a plurality of glycerin, ethylene glycol or polyvinyl alcohol.
The silicon carbide particle catcher prepared by the preparation method has the thermal expansion coefficient of less than or equal to 4.0 x 10 under the condition that the highest sintering temperature is 1500 DEG C -6 /℃。
The beneficial effects are that:
(1) The invention provides a silicon carbide particle catcher, which takes silicon carbide coarse powder and metal silicon powder as main raw materials, wherein strontium doped glass powder is added into the silicon carbide coarse powder, and the addition of a low-melting glass phase can inhibit the silicon carbideThe cristobalization of silicon dioxide greatly reduces the thermal expansion coefficient of the silicon carbide product, and the thermal expansion coefficient of the silicon carbide prepared by inspection under the condition that the highest sintering temperature is 1500 ℃ is less than or equal to 4.0 x 10 -6 /℃。
(2) The invention provides a silicon carbide particle catcher, which optimizes the strontium doping content in strontium doped borosilicate glass powder and determines that the strontium doping content is 5-10 percent so as to lead the finally sintered silicon carbide to finally obtain lower thermal expansion coefficient.
Detailed Description
The present invention will be further described in detail with reference to examples, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
Example 1:
a method for preparing a silicon carbide particle catcher, comprising the following steps:
(1) Preparation of mixture I: the weight percentage is 4:1, evenly mixing silicon carbide coarse powder and metal silicon powder to obtain a mixture I;
(2) Preparing a mixture II: taking 99 weight percent of mixture I, adding 1 weight percent of sintering aid strontium-doped borosilicate glass powder (the strontium content is 10 percent) into the mixture I, and uniformly mixing to obtain mixture II;
(3) Preparation of mixture III: adding 2 weight percent of corn starch, 5 weight percent of methyl cellulose, 2 weight percent of glycerol and 17 weight percent of deionized water into the mixture II for wet mixing to obtain a mixture III;
(4) Putting the mixture III into a vacuum pugging machine for pugging for 2 hours to form a plastic mud blank;
(5) The plastic mud blank is put into an extruder, and a square honeycomb mud blank unit with a cross section of 38mm x 38mm and 43 holes/square centimeter is formed under the guidance of a die. And then the honeycomb mud blank units are put into a microwave drying oven for drying and shaping, and then cross hole sealing is carried out. Finally, the mixture is put into a high-temperature atmosphere sintering furnace, heated to 1500 ℃ according to a certain sintering curve, kept for 2 hours, and naturally cooled to obtain the silicon carbide ceramic unit.
Example 2:
a method for preparing a silicon carbide particle catcher, comprising the following steps:
(1) Preparation of mixture I: the weight percentage is 4:1, evenly mixing silicon carbide coarse powder and metal silicon powder to obtain a mixture, and taking 98 weight percent of mixture I;
(2) Preparing a mixture II: adding 2 weight percent of sintering aid strontium doped borosilicate glass powder (the strontium content is 6 percent) into the mixture, and uniformly mixing the mixture to obtain a mixture II;
(3) Preparation of mixture III: adding 3 weight percent of corn starch, 6 weight percent of methylcellulose, 3 weight percent of glycerol and 18 weight percent of deionized water into the mixture II for wet mixing to obtain a mixture III;
(4) And (3) putting the mixture III into a vacuum pugging machine for mixing for 2 hours to form a plastic mud blank. The plastic mud blank is put into an extruder, and a square honeycomb mud blank unit with a cross section of 38mm x 38mm and 43 holes/square centimeter is formed under the guidance of a die. And then the honeycomb mud blank units are put into a microwave drying oven for drying and shaping, and then cross hole sealing is carried out. Finally, the mixture is put into a high-temperature atmosphere sintering furnace, heated to 1500 ℃ according to a certain sintering curve, kept for 2 hours, and naturally cooled to obtain the silicon carbide ceramic unit.
Example 3:
a method for preparing a silicon carbide particle catcher, comprising the following steps:
(1) Preparation of mixture I: the weight percentage is 4:1, evenly mixing coarse silicon carbide powder and metal silicon powder to obtain a mixture I;
(2) Preparing a mixture II: taking 97 weight percent of mixture I, adding 3 weight percent of sintering aid strontium-doped borosilicate glass powder (the strontium content is 8 percent) into the mixture I, and uniformly mixing to obtain a mixture II;
(3) Preparation of mixture III: adding 2 weight percent of corn starch, 5 weight percent of methyl cellulose, 4 weight percent of glycerol and 16 weight percent of deionized water into the mixture II for wet mixing to obtain a mixture III;
(4) And (3) putting the mixture III into a vacuum pugging machine for mixing for 2 hours to form a plastic mud blank. The plastic mud blank is put into an extruder, and a square honeycomb mud blank unit with a cross section of 38mm x 38mm and 43 holes/square centimeter is formed under the guidance of a die. And then the honeycomb mud blank units are put into a microwave drying oven for drying and shaping, and then cross hole sealing is carried out. Finally, the mixture is put into a high-temperature atmosphere sintering furnace, heated to 1500 ℃ according to a certain sintering curve, kept for 2 hours, and naturally cooled to obtain the silicon carbide ceramic unit.
Example 4:
a method for preparing a silicon carbide particle catcher, comprising the following steps:
(1) Preparation of mixture I: the weight percentage is 4:1, evenly mixing coarse silicon carbide powder and metal silicon powder to obtain a mixture I;
(2) Preparing a mixture II: taking 95 weight percent of mixture I, adding 5 weight percent of sintering aid strontium-doped borosilicate glass powder (the strontium content is 5 percent) into the mixture I, and uniformly mixing to obtain mixture II;
(3) Preparation of mixture III: adding 3 weight percent of corn starch, 6 weight percent of methylcellulose, 3 weight percent of glycerol and 17 weight percent of deionized water into the mixture II for wet mixing to obtain a mixture III;
(4) The mixture III is then put into a vacuum pugging machine for mixing for 2 hours to form a plastic mud blank. The plastic mud blank is put into an extruder, and a square honeycomb mud blank unit with a cross section of 38mm x 38mm and 43 holes/square centimeter is formed under the guidance of a die. And then the honeycomb mud blank units are put into a microwave drying oven for drying and shaping, and then cross hole sealing is carried out. Finally, the mixture is put into a high-temperature atmosphere sintering furnace, heated to 1500 ℃ according to a certain sintering curve, kept for 2 hours, and naturally cooled to obtain the silicon carbide ceramic unit.
Comparative example:
the weight percentage is 4:1 and metal silicon powder to obtain a mixture, taking 100 weight percent of mixture I, adding 2 weight percent of corn starch, 5 weight percent of methylcellulose, 2 weight percent of glycerol and 18 weight percent of deionized water into the mixture to carry out wet mixing, and then putting the mixture into a vacuum pugging machine to carry out pugging for 2 hours to form a plastic mud blank. The plastic mud blank is put into an extruder, and a square honeycomb mud blank unit with a cross section of 38mm x 38mm and 43 holes/square centimeter is formed under the guidance of a die. And then the honeycomb mud blank units are put into a microwave drying oven for drying and shaping, and then cross hole sealing is carried out. Finally, the mixture is put into a high-temperature atmosphere sintering furnace, heated to 1500 ℃ according to a certain sintering curve, kept for 2 hours, and naturally cooled to obtain the silicon carbide ceramic unit.
The silicon carbide ceramic units prepared in examples 1 to 4 and comparative example were subjected to a thermal expansion coefficient test, and the test results are shown in the following table:
the test proves that the addition of the sintering aid obviously reduces the thermal expansion coefficient of the silicon carbide ceramic unit, and the silicon carbide ceramic unit is suitable for being used in a severe motor vehicle environment.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (1)
1. The preparation method of the silicon carbide particle catcher is characterized by comprising the following steps of:
s1, preparing a mixture I: mixing coarse silicon carbide powder and metal silicon powder according to a certain proportion to obtain a mixture I;
s2, preparing a mixture II: taking 95-99% of mixture I and 1-5% of sintering aid, and uniformly mixing to obtain mixture II;
s3, preparing a mixture III: adding 2-3% of pore-forming agent, 5-6% of binder, 2-4% of plasticizer and 16-18% of solvent into the mixture II for wet mixing to obtain a mixture III;
s4: putting the mixture III into a vacuum pugging machine for pugging to form a shaping mud blank;
s5: putting the shaped mud blank formed in the step S4 into an extruder, and forming a square honeycomb mud blank unit under the action of a die;
s6: putting the square honeycomb mud blank unit prepared in the step S5 into a microwave drying oven for drying and shaping, and then carrying out cross hole sealing to obtain a silicon carbide blank unit;
s7: putting the monomer biscuit obtained in the step S6 into a high-temperature atmosphere sintering furnace, heating and preserving heat according to a certain sintering curve, and naturally cooling after the heat preservation is finished to obtain a silicon carbide unit;
s8: bonding a plurality of silicon carbide units obtained in the step S7 into a whole by using an inorganic bonding material, and drying, excircle processing and skin grafting to obtain the silicon carbide particle catcher;
in the S1, the weight percentage of the silicon carbide coarse powder to the metal silicon powder is 4:1, S7, wherein the heating temperature is 1300-1700 ℃, the heat preservation time is 1.5-3 h, the sintering aid in S2 is strontium doped borosilicate glass powder, the strontium content is 5-10%, the pore-forming agent is one or a mixture of more of corn starch, wheat starch and sweet potato starch, the binder is one or a mixture of two of methyl cellulose and ethyl cellulose, the plasticizer is one or a mixture of more of glycerol, ethylene glycol or polyvinyl alcohol, and the thermal expansion coefficient of the silicon carbide particles at the highest sintering temperature of 1500 ℃ is less than or equal to 4.0 multiplied by 10 -6 /℃。
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