CN102172449A - Method for preparing silicon nitride particulate filter - Google Patents
Method for preparing silicon nitride particulate filter Download PDFInfo
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- CN102172449A CN102172449A CN2010106179591A CN201010617959A CN102172449A CN 102172449 A CN102172449 A CN 102172449A CN 2010106179591 A CN2010106179591 A CN 2010106179591A CN 201010617959 A CN201010617959 A CN 201010617959A CN 102172449 A CN102172449 A CN 102172449A
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Abstract
The invention relates to a method for preparing a silicon nitride particulate filter, which comprises the following process steps of: (1) mixing silicon nitride and a sintering aid to obtain mixed powder; (2) sequentially adding a binder, water and a lubricant into the mixed powder, stirring and carrying out mud refining to obtain mud with plasticity; (3) placing the mud into a honeycomb ceramic die and carrying out extrusion forming in an extruding machine to obtain a honeycomb ceramic green body; (4) drying the honeycomb ceramic green body and carrying out latex drainage on the dried honeycomb ceramic green body under the air atmosphere; (5) placing the honeycomb ceramic green body subjected to latex drainage into a sintering furnace, and sintering to obtain silicon nitride honeycomb ceramic; and (6) and alternately blocking up holes at both ends of honeycomb pore passages adjacent to the silicon nitride honeycomb ceramic to obtain the silicon nitride particulate filter. By the method, the silicon nitride diesel particulate filter (DPF) with high cost performance can be prepared, the porosity of a material can be improved, the maximum gas permeability and the minimum pressure drop are obtained, and the economy of fuel oil is improved.
Description
Technical field
The present invention relates to a kind of particle trapper, especially a kind of preparation method of wall-flow type silicon nitride material particle trapper.
Background technology
Because diesel engine has good economy and dynamic property, obtains application more and more widely in recent years on motor vehicle.But diesel vehicle in use discharges a large amount of particulates and nitrogen oxide.The main component of particulate is a carbon because its particle diameter is very little, can be suspended in for a long time aerial, serious environment pollution, and human body had strong carcinogenesis.Therefore, world many countries has successively been formulated the rules of restriction small particle emission of diesel car.The Europe and the U.S. began heavy-duty diesel vehicle has been implemented strict Europe V and EPA2010 discharge standard respectively at 2008 and 2010.
Diesel engine particle catcher (DPF) also claim particulate filter, can reduce its discharging by the particulate in the multiple filtration mechanism capture tail gas.Along with the growth of working time, the particulate of DPF inner accumulated increases, and must these particulates be removed with renovation process such as burnings.At present, developed country generally adopts the honeycomb ceramic filter of extrusion modling as the main version of DPF.It axially has many parallel honeycomb ducts, and adjacent two ends, honeycomb duct are alternately stopped up.This structure forces diesel exhaust gas to enter from the import duct that enters the mouth unlimited, and the ceramic wall that passes porous enters the duct that adjacent outlet is opened wide, and particulate just is deposited on the wall in each import duct, so be referred to as honeycomb ceramic filter.The key technology of wall-flow type DPF is material, because harsh regenerative environ-ment, that the material that constitutes DPF should have is high temperature resistant, thermal coefficient of expansion is low, thermal conductivity is high and a series of performances such as corrosion resistance and mechanical strength excellence.
The current material that generally adopts carborundum as wall-flow type DPF, carborundum has many advantages such as maximum operation temperature height, thermal conductivity height, good corrosion resistance, but the sintering temperature of carborundum is usually more than 2000 ℃, and preparation cost is very high; Thermal coefficient of expansion is also higher in addition, and structure need be made the form of dividing body assembly unit, and cost is further risen.Cordierite also has a spot of application on DPF, cordierite low price, thermal coefficient of expansion are very low, but thermal conductivity, maximum operation temperature, mechanical strength are all lower, the phenomenon that partial melting destroys takes place during regeneration easily, and corrosion resistance is also relatively poor.
In order to overcome above-mentioned two kinds of existing problems of material, silicon nitride has obtained researcher's attention as a kind of candidate material of DPF, owing in the microstructure after burning till a large amount of bar-shaped β-Si are arranged
3N
4The existence of crystal grain, the outstanding advantage of silicon nitride DPF are also to have gratifying intensity when having high porosity.This means that under the prerequisite that proof strength meets the demands pressure drop reduces in the time of can making work by the porosity that improves DPF, improves fuel economy.Because the thermal coefficient of expansion of silicon nitride and thermal conductivity are between cordierite and carborundum, Young's modulus is lower, and the thermal shock resistance excellence does not need the monolithic construction DPF cut apart so can make one.Its corrosion resistance excellence obviously is better than cordierite in addition.(AsahiGlass Co. Ltd) has reported that with relatively inexpensive silica flour be raw material, prepares silicon nitride DPF by the nitridation reaction sintering, and this method has reduced the preparation cost of silicon nitride DPF in Japan AGC company.But because nitridation reaction was difficult to carry out bar-shaped β-Si among this DPF fully in the later stage
3N
4The shared ratio of crystal grain is not high, thereby the performance of the many excellences of silicon nitride can't farthest embody.At present the silicon nitride DPF by Si powder nitrogenize preparation does not still have an application commercial.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of silicon nitride material particle trapper is provided, cost is lower, can obtain the silicon nitride trap of high-performance, height cost performance.
According to technical scheme provided by the invention, the preparation method of described silicon nitride material particle trapper, its component ratio is counted by weight, comprises following processing step:
(1) 90～98 parts silicon nitride and 2～10 parts sintering aid mixing are obtained mixed-powder;
(2) in the mixed-powder that step (1) obtains, add 5～20 parts binding agent, 20～30 parts water and 1～10 part lubricant successively, stir pugging and obtain compliant pug, described mixing speed is 20～100 rev/mins, and mixing time is 0.5～1.5 hour;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 0.5～1.5MPa; The cellular densities of described ceramic honey comb green compact is 100～300 order/square inches;
(4) the ceramic honey comb green compact that step (3) is obtained are under 30～60 ℃ condition dry 2～6 hours; Dried ceramic honey comb green compact are warming up to 500～600 ℃ under air atmosphere, are incubated 0.5～2 hour and carry out binder removal, described programming rate is 0.5～1 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1700～1850 ℃, be incubated 1～3 hour, obtain the silicon nitride honeycomb pottery with 5 ℃～10 ℃/minute programming rates; Described nitrogen gas pressure is 0.1～0.6MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Described sintering aid is Y
2O
3, Al
2O
3Or one or more mixtures among the MgO.
Described binding agent is organic binder bond and/or inorganic binder, and described organic binder bond is methylcellulose, hydroxypropyl methylcellulose, starch or dextrin, and described inorganic binder is the high-ductility bentonite.
Described lubricant is vegetable oil or animal oil.
Described lubricant is soya-bean oil, castor oil or lard.
The purity of described silicon nitride is 90%～99%, and the average grain diameter of silicon nitride is 0.5～5 micron.
The invention has the beneficial effects as follows, according to method of the present invention, form by adjusting prescription, can make high performance-price ratio silicon nitride DPF with different technologies index, can improve the material porosity as far as possible, obtain maximum gas permeability and minimum pressure drop, improve fuel economy, material still has enough intensity to satisfy instructions for use simultaneously.This silicon nitride DPF is used for diesel vehicle, will significantly reduce the discharge capacity of particulate in the exhaust gas from diesel vehicle, makes it to satisfy the Abgasgesetz of increasingly stringent.It is that primary raw material makes silicon nitride DPF that the present invention utilizes the alpha-silicon nitride powders than low-purity (90%～99%), because the purity of the alpha-silicon nitride powders of being taked is lower than expensive high-purity (more than 99%) alpha-silicon nitride powders, so preparation cost can obviously reduce.Owing to still have a large amount of bar-shaped β-Si in the microstructure of alpha-silicon nitride powders after burning till than low-purity
3N
4Crystal grain exists, so series of advantages such as that the silicon nitride DPF that finally makes still has is high temperature resistant, corrosion-resistant, good thermal shock, mechanical strength height.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment.
The purity of alpha-silicon nitride powders used in the present invention is generally 90～99%, preferentially selects 93～97%.If less than 90%, impurity is too many in the alpha-silicon nitride powders, influences sintering character, and the performance that finally makes DPF is compared with carborundum, will not have advantage; If greater than 99%, the preparation cost of alpha-silicon nitride powders obviously rises, and causes the final corresponding increase of silicon nitride DPF cost, is unfavorable for the large-scale application of silicon nitride DPF.It is 0.5～5 micron that the average grain diameter of alpha-silicon nitride powders requires, and preferentially selects 1～3 micron, if greater than 5 microns, sintering velocity is obviously slack-off, and sintering time increases, and preparation cost obviously rises; If less than 0.5 micron, cost of material can obviously increase.The consumption of alpha-silicon nitride powders is too low among the present invention, and then sintering aid is too much, and the porosity of porous silicon nitride is too low behind the sintering, and the intergranular phase content is too much, influences serviceability; If consumption is too high, then sintering aid is very few, bar-shaped β-Si behind the sintering
3N
4Crystal grain is difficult to growth fully, and the intensity of porous silicon nitride reduces.
Sintering aid among the present invention is meant the metal oxide that is varied to glassy phase in the high temperature field of sintering, comprises that also a kind of oxide of or several compositions can become the mixture of glassy phase by reaction.The sintering aid that the present invention uses is Y
2O
3, Al
2O
3Or among the MgO one or more, sintering aid is too high or too low all to have harmful effect to the performance of burning till the back porous silicon nitride.
Binder removal step of the present invention is for organic matters such as the binding agent that adds in the binder removal removal ceramic honey comb green compact, lubricants, as methylcellulose, hydroxypropyl methylcellulose, starch, castor-oil plant wet goods.
The green compact of preparation method of the present invention behind binder removal are put into sintering furnace and carried out the step that sintering obtains the silicon nitride honeycomb pottery, and the sintering nitrogen pressure is 0.1～0.6MPa, and nitrogen pressure is too low, and silicon nitride volatilizees easily, and are weightless excessive; Nitrogen pressure is too high, and final base substrate is densified easily, and the porosity that obtains is too low.Too high or the long crystal grain that all can cause of temperature retention time of temperature is too grown up during sintering, and the silicon nitride grain draw ratio is diminished, and influences final mechanical strength, and causes unnecessary energy waste; And sintering temperature is crossed low or the too short meeting of temperature retention time causes and can't generate bar-shaped silicon nitride grain or crystal grain ateliosis, can influence the performance of final material equally.At last the ceramic honey comb behind the sintering is replaced plug-hole and obtain silicon nitride DPF.
Embodiment one: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 95 parts of purity be 90%, average grain diameter is 2 microns silicon nitride and 5 parts sintering aid Y
2O
3Mix and obtain mixed-powder;
(2) in the mixed-powder that step (1) obtains, add 5 parts binding agent methylcellulose, 20 parts water and 1 part lubricant soya-bean oil successively, stir pugging and obtain compliant pug, described mixing speed is 20 rev/mins, and mixing time is 0.5 hour;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 0.5MPa; The cellular densities of described ceramic honey comb green compact is 100 order/square inches;
(4) the ceramic honey comb green compact that step (3) is obtained are under 30 ℃ condition dry 2 hours; Dried ceramic honey comb green compact are warming up to 500 ℃ under air atmosphere, are incubated 0.5 hour and carry out binder removal, described programming rate is 0.5 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1750 ℃, be incubated 1 hour, obtain the silicon nitride honeycomb pottery with 5 ℃/minute programming rates; Described nitrogen gas pressure is 0.1MPa; Described nitrogen gas purity is 99.999%.
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Embodiment two: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 95 parts of purity be 93%, average grain diameter is 2 microns silicon nitride and 5 parts sintering aid MgO mixes and obtains mixed-powder;
(2) in the mixed-powder that step (1) obtains, add 20 parts binding agent hydroxypropyl methylcellulose, 30 parts water and 10 parts lubricant castor oil successively, stir pugging and obtain compliant pug, described mixing speed is 100 rev/mins, and mixing time is, 1.5 hours;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 1.5MPa; The cellular densities of described ceramic honey comb green compact is 300 order/square inches;
(4) under the condition of 60 ℃ on ceramic honey comb green compact that step (3) is obtained dry 6 hours; Dried ceramic honey comb green compact are warming up to 600 ℃ under air atmosphere, are incubated 2 hours and carry out binder removal, described programming rate is 1 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1750 ℃, be incubated 1 hour, obtain the silicon nitride honeycomb pottery with 10 ℃/minute programming rates; Described nitrogen gas pressure is 0.1MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Embodiment three: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 98 parts of purity be 93%, average grain diameter is 5 microns silicon nitride and 2 parts sintering aid Y
2O
3Mix and obtain mixed-powder;
(2) add 6 parts adhesive starch, 21 parts water and 2 parts lubricant lard successively in the mixed-powder that step (1) obtains, stir pugging and obtain compliant pug, described mixing speed is 30 rev/mins, and mixing time is 1 hour;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 1MPa; The cellular densities of described ceramic honey comb green compact is 120 order/square inches;
(4) under the condition of 40 ℃ on ceramic honey comb green compact that step (3) is obtained dry 3 hours; Dried ceramic honey comb green compact are warming up to 550 ℃ under air atmosphere, are incubated 1 hour and carry out binder removal, described programming rate is 0.6 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1750 ℃, be incubated 1 hour, obtain the silicon nitride honeycomb pottery with 6 ℃/minute programming rates; Described nitrogen gas pressure is 0.1MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Embodiment four: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 90 parts of purity be 96%, average grain diameter is 1 micron silicon nitride, 5 parts sintering aid Y
2O
3Obtain mixed-powder with 5 parts sintering aid MgO mixing;
(2) add 7 parts binding agent dextrin, 22 parts water and 3 parts lubricant soya-bean oil successively in the mixed-powder that step (1) obtains, stir pugging and obtain compliant pug, described mixing speed is 40 rev/mins, and mixing time is 0.7 hour;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 0.7MPa; The cellular densities of described ceramic honey comb green compact is 130 order/square inches;
(4) under the condition of 50 ℃ on ceramic honey comb green compact that step (3) is obtained dry 4 hours; Dried ceramic honey comb green compact are warming up to 520 ℃ under air atmosphere, are incubated 0.7 hour and carry out binder removal, described programming rate is 0.7 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1750 ℃, be incubated 2 hours, obtain the silicon nitride honeycomb pottery with 7 ℃/minute programming rates; Described nitrogen gas pressure is 0.1MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Embodiment five: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 95 parts of purity be 96%, average grain diameter is 2 microns silicon nitride, 2 parts sintering aid Y
2O
3Sintering aid Al with 3 parts
2O
3Mix and obtain mixed-powder;
(2) in the mixed-powder that step (1) obtains, add 8 parts binding agent high-ductility bentonite, 23 parts water and 4 parts lubricant castor oil successively, stir pugging and obtain compliant pug, described mixing speed is 50 rev/mins, and mixing time is 0.8 hour;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 0.8MPa; The cellular densities of described ceramic honey comb green compact is 140 order/square inches;
(4) under the condition of 35 ℃ on ceramic honey comb green compact that step (3) is obtained dry 5 hours; Dried ceramic honey comb green compact are warming up to 530 ℃ under air atmosphere, are incubated 0.8 hour and carry out binder removal, described programming rate is 0.8 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1800 ℃, be incubated 2 hours, obtain the silicon nitride honeycomb pottery with 8 ℃/minute programming rates; Described nitrogen gas pressure is 0.6MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Embodiment six: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 95 parts of purity be 96%, average grain diameter is 2 microns silicon nitride and 5 parts sintering aid Y
2O
3Mix and obtain mixed-powder;
(2) add 9 parts binding agent methylcellulose, 24 parts water and 4 parts lubricant lard successively in the mixed-powder that step (1) obtains, stir pugging and obtain compliant pug, described mixing speed is 60 rev/mins, and mixing time is 1 hour;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 1.2MPa; The cellular densities of described ceramic honey comb green compact is 200 order/square inches;
(4) under the condition of 50 ℃ on ceramic honey comb green compact that step (3) is obtained dry 4 hours; Dried ceramic honey comb green compact are warming up to 560 ℃ under air atmosphere, are incubated 1.6 hours and carry out binder removal, described programming rate is 0.8 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1800 ℃, be incubated 2 hours, obtain the silicon nitride honeycomb pottery with 9 ℃/minute programming rates; Described nitrogen gas pressure is 0.3MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Embodiment seven: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 95 parts of purity be 99%, average grain diameter is 0.5 micron silicon nitride and 5 parts sintering aid MgO mixes and obtains mixed-powder;
(2) in the mixed-powder that step (1) obtains, add 10 parts binding agent hydroxypropyl methylcellulose, 25 parts water and 6 parts lubricant lard successively, stir pugging and obtain compliant pug, described mixing speed is 60 rev/mins, and mixing time is 1.2 hours;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 0.9MPa; The cellular densities of described ceramic honey comb green compact is 180 order/square inches;
(4) under the condition of 45 ℃ on ceramic honey comb green compact that step (3) is obtained dry 4 hours; Dried ceramic honey comb green compact are warming up to 580 ℃ under air atmosphere, are incubated 1.6 hours and carry out binder removal, described programming rate is 0.9 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1850 ℃, be incubated 2 hours, obtain the silicon nitride honeycomb pottery with 9 ℃/minute programming rates; Described nitrogen gas pressure is 0.3MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Embodiment eight: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 95 parts of purity be 99%, average grain diameter is 1 micron silicon nitride, 3 parts sintering aid Y
2O
3Sintering aid Al with 2 parts
2O
3Mix and obtain mixed-powder;
(2) add 10 parts adhesive starch, 28 parts water and 9 parts lubricant soya-bean oil successively in the mixed-powder that step (1) obtains, stir pugging and obtain compliant pug, described mixing speed is 80 rev/mins, and mixing time is 1.5 hours;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 1.5MPa; The cellular densities of described ceramic honey comb green compact is 300 order/square inches;
(4) under the condition of 60 ℃ on ceramic honey comb green compact that step (3) is obtained dry 6 hours; Dried ceramic honey comb green compact are warming up to 600 ℃ under air atmosphere, are incubated 2 hours and carry out binder removal, described programming rate is 1 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1700 ℃, be incubated 2 hours, obtain the silicon nitride honeycomb pottery with 10 ℃/minute programming rates; Described nitrogen gas pressure is 0.6MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
Embodiment nine: a kind of preparation method of silicon nitride material particle trapper, and its component ratio is counted by weight, comprises following processing step:
(1) with 98 parts of purity be 99%, average grain diameter is 3 microns silicon nitride and 2 parts sintering aid Al
2O
3Mix and obtain mixed-powder;
(2) add 18 parts binding agent dextrin, 25 parts water and 8 parts lubricant castor oil successively in the mixed-powder that step (1) obtains, stir pugging and obtain compliant pug, described mixing speed is 50 rev/mins, and mixing time is 1 hour;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 1MPa; The cellular densities of described ceramic honey comb green compact is 200 order/square inches;
(4) under the condition of 50 ℃ on ceramic honey comb green compact that step (3) is obtained dry 5 hours; Dried ceramic honey comb green compact are warming up to 550 ℃ under air atmosphere, are incubated 1 hour and carry out binder removal, described programming rate is 0.6 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1700 ℃, be incubated 3 hours, obtain the silicon nitride honeycomb pottery with 6 ℃/minute programming rates; Described nitrogen gas pressure is 0.6MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
The resulting silicon nitride material of the present invention particle trapper is carried out scanning electron microscope observation, can find, under different component prescription and sintering process condition, a large amount of bar-shaped β-Si are arranged all in the microstructure
3N
4Crystal grain forms, but the draw ratio and the porosity all have bigger difference, shows to adjust the microstructure of silicon nitride DPF by changing technological parameter.
The raw material of silicon nitride DPF composition and sintering condition are as shown in table 1 in the various embodiments of the present invention.
For the silicon nitride DPF that preparation method of the present invention obtains, three-point bending strength, Archimedes's drainage mensuration open pore rate, the mercury injection method measured under the room temperature are tested average air vent aperture; Measured results such as open pore rate, air vent aperture and three-point bending strength are as shown in table 2.
The raw material of table 1 silicon nitride DPF is formed and sintering condition
The main performance of the silicon nitride DPF that table 2 the present invention obtains
| Open pore rate (%) | Average pore size (um) | Bending strength (MPa) | |
| Embodiment 1 | 45 | 0.6 | 163 |
| Embodiment 2 | 50 | 0.8 | 120 |
| Embodiment 3 | 60 | 1.1 | 72 |
| Embodiment 4 | 36 | 0.5 | 215 |
| Embodiment 5 | 46 | 0.6 | 172 |
| Embodiment 6 | 40 | 0.6 | 186 |
| Embodiment 7 | 48 | 0.8 | 98 |
| Embodiment 8 | 42 | 0.7 | 170 |
| Embodiment 9 | 54 | 0.9 | 87 |
As can be seen from Table 2 at the nitrogen atmosphere of 0.1～0.6MPa, in 1700～1850 ℃ the temperature range during sintering, the sample of different material prescription can obtain 36%～60% open pore rate, shown very high bending strength simultaneously, reach as high as 215MPa, under the same porosity, intensity is apparently higher than the cordierite and the silicon carbide material of current use.
Claims (5)
1. the preparation method of a silicon nitride material particle trapper, it is characterized in that: its component ratio is counted by weight, comprises following processing step:
(1) 90～98 parts silicon nitride and 2～10 parts sintering aid mixing are obtained mixed-powder;
(2) in the mixed-powder that step (1) obtains, add 5～20 parts binding agent, 20～30 parts water and 1～10 part lubricant successively, stir pugging and obtain compliant pug, described mixing speed is 20～100 rev/mins, and mixing time is 0.5～1.5 hour;
(3) pug that step (2) is obtained is put into the ceramic honey comb mould, and extrusion molding obtains the ceramic honey comb green compact in extruder, and the extruding force of extruder is 0.5～1.5MPa; The cellular densities of described ceramic honey comb green compact is 100～300 order/square inches;
(4) under the condition of 30～60 ℃ on ceramic honey comb green compact that step (3) is obtained dry 2～6 hours; Dried ceramic honey comb green compact are warming up to 500～600 ℃ under air atmosphere, are incubated 0.5～2 hour and carry out binder removal, described programming rate is 0.5～1 ℃/minute;
(5) will put into sintering furnace through the ceramic honey comb green compact behind step (4) binder removal, charge into nitrogen, be warming up to 1700～1850 ℃, be incubated 1～3 hour, obtain the silicon nitride honeycomb pottery with 5 ℃～10 ℃/minute programming rates; Described nitrogen gas pressure is 0.1～0.6MPa;
(6) the adjacent two ends, honeycomb duct of silicon nitride honeycomb pottery that step (5) obtained replace plug-hole, obtain described silicon nitride material particle trapper.
2. the preparation method of a kind of silicon nitride material particle trapper as claimed in claim 1 is characterized in that: described sintering aid is Y
2O
3, Al
2O
3Or one or more mixtures among the MgO.
3. the preparation method of a kind of silicon nitride material particle trapper as claimed in claim 1, it is characterized in that: described binding agent is organic binder bond and/or inorganic binder, described organic binder bond is methylcellulose, hydroxypropyl methylcellulose, starch or dextrin, and described inorganic binder is the high-ductility bentonite.
4. the preparation method of a kind of silicon nitride material particle trapper as claimed in claim 1 is characterized in that: described lubricant is vegetable oil or animal oil.
5. the preparation method of a kind of silicon nitride material particle trapper as claimed in claim 4 is characterized in that: described lubricant is soya-bean oil, castor oil or lard.
The preparation method of 6 a kind of silicon nitride material particle trappers as claimed in claim 1 is characterized in that: the purity of described silicon nitride is 90%～99%, and the average grain diameter of silicon nitride is 0.5～5 micron.
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| CN2010106179591A Pending CN102172449A (en) | 2010-12-31 | 2010-12-31 | Method for preparing silicon nitride particulate filter |
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| CN104072148A (en) * | 2013-03-29 | 2014-10-01 | 北京市理化分析测试中心 | Low-cost preparation method of silicon nitride honeycomb ceramics |
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| CN114352380A (en) * | 2022-01-10 | 2022-04-15 | 岚士智能科技(上海)有限公司 | Processing method and equipment of silicon carbide DPF |
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| CN115466132A (en) * | 2021-06-10 | 2022-12-13 | 阜阳师范大学 | Method for preparing silicon nitride honeycomb ceramic |
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| CN103508749A (en) * | 2012-06-18 | 2014-01-15 | 苏州忠辉蜂窝陶瓷有限公司 | Extrusion molding method for preparing silicon nitride honeycomb ceramic |
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| CN114352380B (en) * | 2022-01-10 | 2022-12-02 | 岚士智能科技(上海)有限公司 | Processing method and equipment of silicon carbide DPF |
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