CN116669830A - 碳化硅陶瓷蜂窝状结构体及其制造方法 - Google Patents
碳化硅陶瓷蜂窝状结构体及其制造方法 Download PDFInfo
- Publication number
- CN116669830A CN116669830A CN202280008608.1A CN202280008608A CN116669830A CN 116669830 A CN116669830 A CN 116669830A CN 202280008608 A CN202280008608 A CN 202280008608A CN 116669830 A CN116669830 A CN 116669830A
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- Prior art keywords
- silicon carbide
- particles
- ceramic honeycomb
- honeycomb structure
- phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000000919 ceramic Substances 0.000 title claims abstract description 65
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 61
- 238000004519 manufacturing process Methods 0.000 title claims description 22
- 239000002245 particle Substances 0.000 claims abstract description 103
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 44
- 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 claims abstract description 44
- 239000011230 binding agent Substances 0.000 claims abstract description 39
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 27
- 239000011029 spinel Substances 0.000 claims abstract description 27
- 238000005192 partition Methods 0.000 claims abstract description 18
- 229910021426 porous silicon Inorganic materials 0.000 claims abstract description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 79
- 239000000395 magnesium oxide Substances 0.000 claims description 50
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 28
- 239000011148 porous material Substances 0.000 claims description 26
- 239000012298 atmosphere Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 15
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 10
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 5
- 239000000347 magnesium hydroxide Substances 0.000 claims description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- 238000005245 sintering Methods 0.000 description 40
- 239000007789 gas Substances 0.000 description 22
- 230000001590 oxidative effect Effects 0.000 description 14
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 13
- 230000035939 shock Effects 0.000 description 13
- 239000010410 layer Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 7
- 229910052753 mercury Inorganic materials 0.000 description 7
- 239000007858 starting material Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000012790 adhesive layer Substances 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 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 4
- 229910052863 mullite Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229910052839 forsterite Inorganic materials 0.000 description 3
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 3
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 3
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 3
- 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 3
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- 238000002459 porosimetry Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007602 hot air drying Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- 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 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229910019440 Mg(OH) Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000001761 ethyl methyl cellulose Substances 0.000 description 1
- 235000010944 ethyl methyl cellulose Nutrition 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 229920013819 hydroxyethyl ethylcellulose Polymers 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
Classifications
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Abstract
一种碳化硅陶瓷蜂窝状结构体具有由多孔碳化硅分隔壁隔开的多个轴向贯通流路,所述分隔壁包括作为骨料的碳化硅粒子和用于粘结所述碳化硅粒子的粘结剂层,所述粘结剂层至少具有堇青石相和尖晶石相,并且所述堇青石相的摩尔比M1[=堇青石相/(堇青石相+尖晶石相)]为0.4‑0.9。
Description
发明领域
本发明涉及一种在陶瓷蜂窝状过滤器中使用的碳化硅陶瓷蜂窝状结构体及其制造方法,所述陶瓷蜂窝状过滤器用于从由内燃机(如柴油机)排放的排气(尾气,exhaustgases)中通过除去粒状物质(其在下文中可以被称为“PM”)来净化排气。
背景技术
因为柴油机的排气中含有的NOx和PM在排放到空气中时可能不利地影响人类和环境,所以已经常规地将携带NOx催化剂的蜂窝状结构体和用于捕获PM的陶瓷蜂窝状过滤器作为排放装置附接至柴油机的排放管。用于通过捕获排气中的PM来净化排气的陶瓷蜂窝状过滤器的一个实例在图1(a)和1(b)中示出。陶瓷蜂窝状过滤器100由以下各项构成:包括形成多个流路13、14的多孔分隔壁12和外周壁11的陶瓷蜂窝状结构体110,以及以棋盘图案交替地密封流出侧密封流路13和流入侧密封流路14的排气引入侧端面15a和排气排放端面15b的上游侧封堵塞16a和下游侧封堵塞16b。如图1(b)中的虚线箭头所示,排气流动到在排气引入侧端面15a上开口的流出侧密封流路13中,通过在分隔壁12之上(表面上)和之中(内部)的连通孔,并且从在排气排出端面15b上开口的流入侧密封流路14排出。在排气通过在分隔壁12之上和之中的连通孔时,排气中的PM被捕获,使得排气被净化。当捕获的PM积累到预定量时,将其燃烧以再生陶瓷蜂窝状过滤器。已知的是,因为这样的陶瓷蜂窝状结构体已经经历了更严酷的使用环境,所以其由具有出色的耐热冲击性的耐火粒子如碳化硅(SiC)粒子形成。
JP 06-182228 A(专利文献1)公开了一种用于制造催化剂载体的方法,该方法包括使用比表面积为0.1-5m2/g且含有1.0-5.0%杂质的碳化硅粉末作为起始材料,将其成型为所需形状,将所得的坯体干燥,然后将其在1600-2200℃的范围内烧结。专利文献1描述了这种方法可以经济地制造具有出色性能的烧结多孔碳化硅的催化剂载体。
JP 06-182228 A中描述的方法仅使用碳化硅粉末作为起始材料来形成烧结体,从碳化硅粒子表面升华的碳化硅组分在粒子之间接触并且积聚,使得粒子彼此粘结。因此,需要极高的烧结温度来形成烧结体,并且在制造具有高孔隙率的过滤器的情况下,这种烧结机制不会充分起作用,从而可能导致低强度。另外,因为这种方法使用通过碳化硅粉末自身的重结晶来粘结碳化硅粒子的烧结机制,所以需要极高的烧结温度,从而导致高成本。
作为一种用于在相对较低的烧结温度下廉价地制造具有足以抑制在用于汽车的排气过滤器时的压力损失的孔隙率且具有高导热性的蜂窝状结构体的方法,JP 2002-201082 A(专利文献2)公开了以下方法。即,JP 2002-201082 A公开了一种用于制造蜂窝状结构体的方法,该方法包括将碳化硅粒子与金属硅和有机粘结剂混合和混炼以形成可成型材料,将该可成型材料成型为蜂窝状,通过煅烧从所得的坯体中除去有机粘结剂,然后烧结该坯体。专利文献2描述了烧结温度优选地在1400-1600℃的范围内,并且在高于或等于氧化开始的温度的温度范围内,烧结气氛优选为非氧化性气氛,如N2、Ar等。
虽然JP 2002-201082 A中所描述的方法可以通过在1400-1600℃的相对较低的温度下烧结来制造具有足以抑制在用作过滤器时的压力损失的孔隙率的蜂窝状结构体,但是烧结理想地在非氧化性气氛中进行以抑制氧化,从而导致用于烧结设施的高成本。
作为一种用于制造尽管孔隙率高但也具有高强度且具有出色的耐热冲击性的碳化硅蜂窝状结构体(其可用于要求具有较高排气透过性的过滤器)的方法,JP 2010-105861A(专利文献3)公开了以下方法。即,JP 2002-201082 A公开了一种用于通过以下方式制造包含1-35质量%的金属硅化物和0.5-10质量%的氧化铝(Al2O3)并且孔隙率为38-80%的多孔碳化硅体的方法:将包含金属、硅、碳源和铝(AL)源的起始材料混合物成型为预定形状,并且将所得的坯体脱脂并烧结。专利文献3描述了烧结温度优选为1250-1800℃,并且烧结气氛优选为惰性气氛。
虽然JP 2010-105861 A中所述的方法可以通过在1250-1800℃的相对较低的温度下烧结来制造具有出色气体透过性和耐热冲击性的多孔碳化硅体,但是烧结应在氩气(Ar)或真空气氛中进行,从而导致烧结设施的高成本。
WO 2013/146954 A(专利文献4)公开了一种孔隙率为40-90%的多孔材料,该多孔材料包含由碳化硅粒子组成的主骨料、由莫来石(mullite)粒子和氧化铝粒子中的至少一种组成的副骨料以及用于粘结骨料的由非晶相和堇青石(cordierite)相中的至少一种组成的粘结剂相。专利文献4描述了可以形成具有改善的耐热冲击性的蜂窝状结构体。JP2002-201082 A中所描述的多孔材料通过以下方式获得:将主骨料碳化硅粉末、副骨料粉末和粘结剂相形成粉末(粘结剂粉末)混合和混炼,并且根据需要加入粘结剂、表面活性剂、孔形成材料、水等,以形成可成型材料,将该可成型材料挤出成型以形成蜂窝状坯体,并且将该坯体干燥并烧结。JP 2002-201082 A描述了烧结优选地在氮气、氩气等的非氧化性气氛中在1300-1600℃下进行。
虽然WO 2013/146954 A中所描述的方法可以通过在1300-1600℃的温度下烧结来制造具有出色的耐热冲击性的多孔材料,但是烧结应在氮气、氩气等的非氧化性气氛中进行,从而导致烧结设施的高成本。
如上所解释的,当耐火粒子如碳化硅(SiC)粒子用作形成用于陶瓷蜂窝状过滤器的陶瓷蜂窝状结构体的材料时,极高的烧结温度和非氧化性气氛是必需的,并且满足这些条件的烧结炉的使用导致高成本。因此,期望开发一种能够更廉价地制造陶瓷蜂窝状结构体的方法。
发明内容
发明目的
因此,本发明的一个目的是提供一种具有足够用于陶瓷蜂窝状过滤器的耐热冲击性的碳化硅陶瓷蜂窝状结构体及其制造方法,该碳化硅陶瓷蜂窝状结构体可以在不需要非氧化性气氛的情况下利用在比先前更低的烧结温度的烧结过程比先前更廉价地制造。
问题的解决方案
鉴于上述目的,本发明人进行了深入的研究以获得即使使用在不需要非氧化性气氛的情况下在比先前更低的烧结温度的烧结过程,也可以保持足够的耐热冲击性的陶瓷蜂窝状结构体。作为结果,本发明人关注起始材料粒子的配制,从而完成了本发明。
因此,具有由多孔碳化硅分隔壁(孔壁或单元格壁,cell wall)隔开的多个轴向贯通流路的本发明的碳化硅陶瓷蜂窝状结构体的特征在于:所述分隔壁包含作为骨料的碳化硅粒子和用于粘结(结合,binding)这些碳化硅粒子的粘结剂层(结合层,binder layer),所述粘结剂层至少具有堇青石相和尖晶石(spinel)相,并且该堇青石相的摩尔比M1[=堇青石相/(堇青石相+尖晶石相)]为0.4-0.9。
在本发明的碳化硅陶瓷蜂窝状结构体中,分隔壁的孔隙率优选为35-50%。
在本发明的碳化硅陶瓷蜂窝状结构体中,分隔壁的中值孔径优选为5-20μm。
本发明的用于制造碳化硅陶瓷蜂窝状结构体的方法包括以下步骤:将碳化硅粒子、至少包含氧化铝源粒子和氧化镁源粒子的粘结剂以及有机粘结剂配制、混合和混炼以形成可成型材料,将该可成型材料挤出成型为蜂窝状,将所得的坯体干燥,然后将该坯体在空气气氛中在1200-1350℃的温度范围内烧结。
在本发明的用于制造碳化硅陶瓷蜂窝状结构体的方法中,氧化铝源粒子和氧化镁源粒子优选地以0.32-0.50的摩尔比M2[=(Al2O3)/(Al2O3+MgO)]配制。
在本发明的用于制造碳化硅陶瓷蜂窝状结构体的方法中,相对于100质量%的碳化硅粒子,氧化铝源粒子和氧化镁源粒子优选总计为6-15质量%。
在本发明的用于制造碳化硅陶瓷蜂窝状结构体的方法中,优选的是,在粘结剂中,氧化铝源粒子为氧化铝或氢氧化铝粒子,并且氧化镁源粒子为氧化镁或氢氧化镁粒子。
发明效果
本发明可以提供一种具有足够用于陶瓷蜂窝状过滤器的耐热冲击性的碳化硅陶瓷蜂窝状结构体及其制造方法,所述碳化硅陶瓷蜂窝状结构体可以在不需要非氧化性气氛的情况下通过利用比先前更低的温度的烧结过程比先前更廉价地制造。
附图说明
图1(a)是示意性示出了陶瓷蜂窝状过滤器的一个实例的正视图。
图1(b)是示意性示出了陶瓷蜂窝状过滤器的一个实例的与轴向平行的部分横截面图。
图2是示意性示出了一种陶瓷蜂窝状段(部分,segment)的透视图。
图3是示意性示出通过一体化接合形成的陶瓷蜂窝状过滤器的一个实例的透视图。
具体实施方式
以下将参照附图解释本发明的实施方案。应注意,本发明不限于以下实施方案,并且可以在本发明的范围内进行调整和改进。
[1]陶瓷蜂窝状结构体
本发明的碳化硅陶瓷蜂窝状结构体具有由多孔碳化硅分隔壁隔开的多个轴向贯通流路,分隔壁包含作为骨料的碳化硅粒子和粘结碳化硅粒子的粘结剂层,该粘结剂层至少包含堇青石相和尖晶石相,并且堇青石相的摩尔比M1[=堇青石相/(堇青石相+尖晶石相)]为0.4-0.9。
因为粘结剂层至少包含堇青石相和尖晶石相,并且因为堇青石相的摩尔比M1[=堇青石相/(堇青石相+尖晶石相)]为0.4-0.9,所以粘结剂层可以具有足够的强度和耐热冲击性。堇青石相的摩尔比M1是由堇青石相的摩尔数和尖晶石相的摩尔数通过式[堇青石相(mol)/(堇青石相(mol)+尖晶石相(mol))]确定的比率。当堇青石相的摩尔比M1小于0.4时,强度低,并且热膨胀系数大,从而导致差的耐热冲击性。另一方面,当堇青石相的摩尔比M1超过0.9时,耐热性变低,且分隔壁具有低孔隙率。堇青石相的摩尔比M1优选为0.45-0.70。除了堇青石相和尖晶石相以外,粘结剂层还可以含有方石英(cristobalite)、莫来石、镁橄榄石(forsterite)和其他晶体相,以及非晶相。
堇青石相的摩尔比M1[=堇青石相/(堇青石相+尖晶石相)]可以如下确定。首先,将经烧结的陶瓷蜂窝状结构体的一部分粉碎成粉末,并使其经历X射线衍射测量以获得粉末衍射图,在该粉末衍射图上确定堇青石的(110)面的峰强度和尖晶石的(311)面的峰强度。利用这些峰强度,计算在整个陶瓷蜂窝状结构体中的堇青石与尖晶石的质量比。利用1mol堇青石的质量为585.0并且1mol尖晶石的质量为142.3,将上述质量比换算为堇青石与尖晶石的摩尔比,从而确定堇青石相相对于堇青石相和尖晶石相的总和的摩尔比M1。
因为分隔壁的孔隙率为35-50%,所以本发明的碳化硅陶瓷蜂窝状结构体可以保持低的压力损失,同时保持高的强度。当孔隙率小于35%时,陶瓷蜂窝状结构体存在大压力损失的问题。另一方面,当孔隙率超过50%时,难以提供具有足够强度的陶瓷蜂窝状结构体。孔隙率的下限优选为38%,并且更优选为40%。另一方面,孔隙率的上限优选为49%,并且更优选为48%。
因为分隔壁的中值孔径为5-20μm,所以本发明的碳化硅陶瓷蜂窝状结构体可以保持高强度。当中值孔径小于5μm时,陶瓷蜂窝状结构体存在大压力损失的问题。另一方面,当中值孔径超过20μm时,难以提供具有足够强度的陶瓷蜂窝状结构体。中值孔径的下限优选为8μm,并且更优选为9μm。另一方面,中值孔径的上限优选为18μm,并且更优选为16μm。
本发明的碳化硅陶瓷蜂窝状结构体可以用作如图2所示的蜂窝状段211,使得通过粘结剂层29将多个蜂窝状段211一体化接合来提供如图3所示的复合碳化硅陶瓷蜂窝状结构体210。在通过粘结剂层29将多个蜂窝状部分211一体化接合后,将所得的复合蜂窝状结构体机器加工成在垂直于其流路的横截面中具有圆形、椭圆形、三角形、矩形或任何其他所需形状的外周,并且将机器加工的外周用涂层材料涂覆以形成外周壁21。
可以通过已知方法以棋盘图案交替地封堵在通过一体化接合形成的碳化硅陶瓷蜂窝状结构体210中的排气引入侧25a或排气排出侧25b上的流路,以提供陶瓷蜂窝状过滤器200。可以在烧结前的坯体或经烧结的蜂窝状段中,或者在它们通过粘结剂层29一体化接合之后,形成流路的封堵塞26a、26b。这些封堵塞可以在排气引入侧或排气排出侧的流路的端面上形成,或在流入侧端面25a或流出侧端面26b内侧的流路的内部中形成。
[2]碳化硅陶瓷蜂窝状结构体的制造方法
将解释说明本发明的碳化硅陶瓷蜂窝状结构体的制造方法的一个实例。
首先,将作为骨料的碳化硅粒子、至少包含氧化铝源粒子和氧化镁源粒子的粘结剂以及有机粘结剂进行配制和混炼。氧化铝源粒子和氧化镁源粒子分别为包含氧化铝的化合物的粒子和包含氧化镁的化合物的粒子,并且它们可以包括包含氧化铝和氧化镁的化合物的粒子。将作为骨料含有的碳化硅粒子通过粘结剂层以形成孔隙的方式粘结。碳化硅粒子的平均粒径优选为30-50μm。
将作为粘结剂的氧化铝源粒子和氧化镁源粒子优选地以0.32-0.50的摩尔比M2[=(Al2O3)/(Al2O3+MgO)]添加。在这样的比率下,粘结剂层可以至少含有堇青石相和尖晶石相。摩尔比M2由所添加的氧化铝源粒子和氧化镁源粒子的质量如下计算。计算氧化铝源粒子中的氧化铝组分(Al2O3)的摩尔数和氧化镁源粒子中的氧化镁组分(MgO)的摩尔数,并且相对于氧化铝组分(Al2O3)和氧化镁组分(MgO)的总摩尔数的氧化铝组分(Al2O3)的摩尔数通过摩尔比M2[=(Al2O3)/(Al2O3+MgO)]表示。
例如,在使用氧化铝[Al(OH)3]作为氧化铝源并且使用氧化镁[Mg(OH)2]作为氧化镁源的情况下,该氧化铝中的氧化铝含量和该氧化镁中的氧化镁含量分别表示为:
Al(OH)3=(1/2)Al2O3+(3/2)H2O,和
Mg(OH)2=MgO+H2O。
相应地,计算出每1mol氧化铝的氧化铝含量为0.5mol,并且计算出每1mol氧化镁的氧化镁含量为1mol。利用这些关系,如上所述地确定氧化铝组分和氧化镁组分的摩尔数,以确定摩尔比M2。类似地,当使用含有氧化铝和氧化镁两者的化合物(例如,尖晶石)的粒子时,计算这种化合物中的氧化铝含量(Al2O3)和氧化镁含量(MgO)以确定摩尔比M2。
当摩尔比M2小于0.32或大于0.50时,耐热冲击性低。摩尔比M2的下限优选为0.35,并且进一步优选为0.40。上限优选为0.48。
相对于100质量%的碳化硅粒子,氧化铝源粒子和氧化镁源粒子的总量优选为6-15质量%。当该总量小于6质量%时,粘结碳化硅粒子的粘结剂层的粘结强度低,从而导致具有低强度的陶瓷蜂窝状结构体。另一方面,当该总量大于15质量%时,耐热冲击性低。相对于100质量%的碳化硅粒子,氧化铝源粒子和氧化镁源粒子的总量的下限优选为7质量%,并且更优选为8质量%。另一方面,并且上限优选为14质量%,并且更优选为13质量%。
氧化铝源粒子的平均粒径优选为1-15μm。氧化镁源粒子的平均粒径优选为1-15μm。
氧化铝源粒子优选为氧化铝或氢氧化铝粒子,并且氧化镁源粒子优选为氧化镁或氢氧化镁粒子。如后面描述的,使用氧化铝或氢氧化铝粒子作为氧化铝源粒子并且使用氧化镁或氢氧化镁粒子作为氧化镁源粒子,烧结可以优选地在不需要非氧化性气氛的情况下在比先前更低的烧结温度下进行。作为粘结剂,特别优选的是使用氧化铝粒子作为氧化铝源粒子并且使用氢氧化镁粒子作为氧化镁源粒子。除了氧化铝源粒子和氧化镁源粒子以外,粘结剂还可以含有尖晶石、莫来石、镁橄榄石等的粒子,它们是氧化铝和/或氧化镁的化合物。
有机粘结剂可以是甲基纤维素、乙基纤维素、乙基甲基纤维素、羧甲基纤维素、羟丙基甲基纤维素、羟乙基纤维素、羟甲基纤维素、羟乙基乙基纤维素等。它们之中,羟丙基甲基纤维素和/或甲基纤维素是优选的。相对于100质量%的可成型材料(碳化硅粒子加粘结剂),有机粘结剂优选为5-15质量%。
然后将混合的起始材料与水混炼以形成增塑的可成型材料。基于起始材料,添加的水的量(被调整以提供具有可成型硬度的可成型材料)优选为20-50质量%。
通过已知的方法经由已知的蜂窝状结构成型模具将所形成的可成型材料挤出成型,以形成蜂窝状结构的坯体。将这种坯体干燥,根据需要在其端面、外周面等进行机器加工,然后在氧化性气氛中在1200-1350℃的温度范围内烧结,以制造碳化硅陶瓷蜂窝状结构体。
虽然没有特别限制,但是干燥方法可以例如是热风干燥、微波加热干燥、高频加热干燥等。
在1200-1350℃的温度范围内,氧化铝源粒子和氧化镁源粒子被烧结而形成粘结碳化硅粒子的粘结剂层。因为烧结可以在这样相对较低的烧结温度下进行,所以可以使用于形成粘结剂层的烧结成本比以前更低。当烧结温度低于1200℃时,粘结剂相不充分地粘结碳化硅粒子,从而无法获得足够的强度。另一方面,当烧结温度高于1350℃时,耐热冲击性低。由于该较低的烧结温度,不需要用于抑制氧化的非氧化性气氛(与常规技术不同),并且烧结可以在氧化性气氛中进行,由此避免了烧结过程中的成本增加。
实施例
以下将参照实施例更详细地解释本发明,同时不意图将本发明局限于此。
实施例1-10以及比较例2和3
将具有表1中所示的粒径的碳化硅粒子和粘结剂粒子(氧化铝源粒子和氧化镁源粒子)以表1中所示的量连同作为有机粘结剂的羟丙基甲基纤维素一起进行配制和混炼。将混合的起始材料与水混炼以形成增塑的可成型材料,将其各自在螺杆成型机中通过蜂窝状结构成型模具挤出,从而形成每条边为34mm的四棱柱形且长度为304mm的蜂窝状结构坯体。将该坯体在热风干燥机中在120℃干燥2小时,并且在氧化性气氛中在1300℃的最高温度下烧结,以获得实施例1-10以及比较例2和3中的各个碳化硅陶瓷蜂窝状结构体(其分隔壁厚度为8密耳(0.20mm)且孔道密度为300cpsi(46.5个孔道/cm2)。
比较例1
除了如表1中所示改变碳化硅粒子和粘结剂粒子的类型和量、在坯体的热风干燥后增加在550℃进行3小时的脱脂步骤以及烧结在氩气气氛中在1450℃的最高温度下进行2小时外,以与实施例1中相同的方式获得比较例1的碳化硅陶瓷蜂窝状结构体。
对于在实施例1-10和比较例1-3的每一个中所获得的碳化硅陶瓷蜂窝状结构体中的一个,如以下所述进行孔隙率、中值孔径、热膨胀系数和A轴抗压强度的测量。结果在表2中示出。
(a)孔隙率和中值孔径的测量
通过水银孔隙率法(压汞法,mercury porosimetry)来进行孔隙率和中值孔径的测量。将从陶瓷蜂窝状结构体中切出的试样(10mm×10mm×10mm)设定在可得自Micromeritics的Autopore III的测量室中,并且将该室排空。之后,在压力下将水银引入到该室中以测定压力与压入到试样的孔隙中的水银的体积之间的关系。将压力换算为孔径,并且将通过从较大侧到较小侧累积孔径确定的累积孔容积(对应于水银的体积)相对于孔径作图,以获得显示出孔径与累积孔容积之间的关系的图。水银引入压力为0.5psi(0.35×10-3kg/mm2),并且用于由压力计算孔径的常数为130°的接触角和484达因/cm的表面张力。在1800psi(1.26kg/mm2,对应于约0.1μm的孔径)的水银压力下的累积孔容积被视为总孔容积。
根据水银孔隙率法测量结果,确定总孔容积和在累积孔容积为总孔容积的50%时的中值孔径。
(b)热膨胀系数的测量
从陶瓷蜂窝状结构体中切出横截面形状为4.5mm×4.5mm且长度为50mm的试样,其纵向方向与流路方向基本上一致,并且以10℃/分钟的升温速度将试样从室温加热到800℃,以通过可得自Rigaku Corp.的ThermoPlus(其为压缩负荷型和差示膨胀型热机械分析仪(TMA))测量在20g的恒定负荷下的纵向长度增加,从而确定在40℃至800℃的平均热膨胀系数。
(c)A轴压缩破坏强度
根据M505-87,日本汽车工程师协会的“用于汽车排气净化催化剂的整体陶瓷载体的测试方法(Test Method of Monolithic Ceramic Carrier for Automobile ExhaustGas Cleaning Catalyst)”,测量从各个陶瓷蜂窝状结构体中切出的直径为24.5mm且长度为24.5mm的试样的A轴压缩破坏强度。
表1
注释:(1)D50表示“中值粒径”。
(2)形成氧化铝源粒子的化合物。
(3)形成氧化镁源粒子的化合物。
(4)摩尔比M2[=(Al2O3)/(Al2O3+MgO)]。
表1(续)
表2
注释:(1)堇青石(摩尔比M1)=堇青石(mol)/[堇青石(mol)+尖晶石(mol)]。
(2)尖晶石(摩尔比)=尖晶石(mol)/[堇青石(mol)+尖晶石(mol)]。
(3)CTE表示“热膨胀系数”。
根据表1和2清楚的是,与比较例1-3相比,本发明中的实施例1-10的陶瓷蜂窝状过滤器更廉价地制造,其耐热性等于或高于比较例1-3的陶瓷蜂窝状过滤器的耐热性,因为它们能够在不需要非氧化性气氛的情况下在更低的最高温度下进行烧结。
Claims (7)
1.一种碳化硅陶瓷蜂窝状结构体,所述碳化硅陶瓷蜂窝状结构体具有由多孔碳化硅分隔壁隔开的多个轴向贯通流路,
所述分隔壁包含作为骨料的碳化硅粒子和用于粘结所述碳化硅粒子的粘结剂层,
所述粘结剂层至少包含堇青石相和尖晶石相,并且
所述堇青石相的摩尔比M1[=堇青石相/(堇青石相+尖晶石相)]为0.4-0.9。
2.根据权利要求1所述的碳化硅陶瓷蜂窝状结构体,其中所述分隔壁的孔隙率为35-50%。
3.根据权利要求1或2所述的碳化硅陶瓷蜂窝状结构体,其中所述分隔壁的中值孔径为5-20μm。
4.一种用于制造根据权利要求1-3所述的碳化硅陶瓷蜂窝状结构体的方法,所述方法包括以下步骤:将碳化硅粒子、包含氧化铝源粒子和氧化镁源粒子的粘结剂以及有机粘结剂配制、混合和混炼以形成可成型材料,将所述可成型材料挤出成型为蜂窝状,将所得的坯体干燥,和将所述坯体在空气气氛中在1200-1350℃的温度范围内烧结。
5.根据权利要求4所述的用于制造碳化硅陶瓷蜂窝状结构体的方法,其中将所述氧化铝源粒子和所述氧化镁源粒子以0.32-0.50的摩尔比M2[=(Al2O3)/(Al2O3+MgO)]进行配制。
6.根据权利要求4或5所述的用于制造碳化硅陶瓷蜂窝状结构体的方法,其中相对于100质量%的所述碳化硅粒子,所述氧化铝源粒子和所述氧化镁源粒子总计为6-15质量%。
7.根据权利要求4-6中任一项所述的用于制造碳化硅陶瓷蜂窝状结构体的方法,其中在所述粘结剂中,所述氧化铝源粒子为氧化铝或氢氧化铝粒子,并且所述氧化镁源粒子为氧化镁或氢氧化镁粒子。
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