WO2007119287A1 - 炭化珪素質多孔体及びその製造方法 - Google Patents
炭化珪素質多孔体及びその製造方法 Download PDFInfo
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- WO2007119287A1 WO2007119287A1 PCT/JP2007/052789 JP2007052789W WO2007119287A1 WO 2007119287 A1 WO2007119287 A1 WO 2007119287A1 JP 2007052789 W JP2007052789 W JP 2007052789W WO 2007119287 A1 WO2007119287 A1 WO 2007119287A1
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- WIPO (PCT)
- Prior art keywords
- silicon
- silicon carbide
- metal
- based porous
- porous material
- Prior art date
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims description 4
- 229910021426 porous silicon Inorganic materials 0.000 title description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 112
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000011148 porous material Substances 0.000 claims abstract description 72
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 35
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000001301 oxygen Substances 0.000 claims abstract description 35
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 35
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 6
- 239000000956 alloy Substances 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract 2
- 229910052751 metal Inorganic materials 0.000 claims description 74
- 239000002184 metal Substances 0.000 claims description 74
- 229910052710 silicon Inorganic materials 0.000 claims description 63
- 239000010703 silicon Substances 0.000 claims description 63
- 238000004519 manufacturing process Methods 0.000 claims description 33
- 229910052782 aluminium Inorganic materials 0.000 claims description 28
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 claims description 16
- 238000007254 oxidation reaction Methods 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000005728 strengthening Methods 0.000 claims 1
- 238000002844 melting Methods 0.000 abstract description 15
- 230000008018 melting Effects 0.000 description 14
- 239000007789 gas Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000002253 acid Substances 0.000 description 7
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000013618 particulate matter Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- -1 conoleto (Co) Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000595 mu-metal Inorganic materials 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24149—Honeycomb-like
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- 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
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249967—Inorganic matrix in void-containing component
- Y10T428/249969—Of silicon-containing material [e.g., glass, etc.]
Definitions
- the present invention relates to a silicon carbide porous body used for automobile exhaust gas purification filters, catalyst carriers, and the like, and a method for producing the same.
- a filter for collecting and removing particulate matter contained in a dust-containing fluid such as diesel engine exhaust gas As a catalyst carrier for carrying a catalyst component for purifying harmful substances in exhaust gas, soot is widely used as a porous hard structure.
- refractory particles such as silicon carbide (SiC) particles are used as a constituent material of such a hard cam structure.
- porous honeycomb structure containing fireproof particles (silicon carbide particles) that are aggregates and metal silicon that is a binder that joins the refractory particles together. Bonded SiC porous body) and a manufacturing method thereof have been proposed (see Patent Document 1).
- the honeycomb structure disclosed in Patent Document 1 can be manufactured at a relatively low firing temperature with a high yield, has a high heat conductivity, is sufficiently porous and has a high specific surface area, and is suitable as a filter or a catalyst carrier. Is available.
- Si when metallic silicon is heated in a low oxygen atmosphere or a reducing atmosphere, Si is volatilized or volatilized as SiO as represented by the following formula (1). It is also known that when these gaseous Si or SiO cause an acid-oxidation reaction or the like, intense heat is generated.
- the generated SiO gas combines with oxygen in the atmosphere to form SiO fibers.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2002-201082
- Patent Document 2 JP 2002-154882 A
- the present invention has been made in view of the above-described problems of the prior art, and its object is to selectively coat only the surface of metal silicon with a compound having a high melting point. It is an object of the present invention to provide a silicon carbide based porous material that can reduce the possibility of oxidation reaction of metallic silicon, improve oxidation resistance, and minimize the decrease in porosity, and a method for producing the same.
- the following silicon carbide based porous body and a method for producing the same are provided.
- phase containing alumina is selected from an alkaline earth metal, rare earth metal, silicon (Si), titanium (Ti), cobalt (Co), and nickel (Ni) forces.
- silicon carbide based porous material according to [1] including the above compound.
- the raw material is calcined at 600 to 1500 ° C. in an inert gas atmosphere or a reduced pressure atmosphere having an oxygen partial pressure of 10_4 atm or less.
- the silicon carbide according to [7] or [8] A method for producing porous bodies.
- the oxygen partial pressure in the oxygen atmosphere is 0.05 atm or higher [7] to [12]
- the silicon carbide based porous material and the method for producing the same of the present invention selectively coats only the surface of metal silicon with a high melting point compound so that the acid-rich reaction of metal silicon occurs. It can reduce the likelihood of occurrence, improve oxidation resistance, and minimize the loss of porosity.
- the silicon carbide based porous material according to the present invention is a silicon carbide in which particles of silicon carbide as an aggregate are bonded together with metal silicon as a binder and with pores held between the silicon carbide particles.
- the surface of the metallic silicon is selectively covered with a phase containing alumina rather than silicon carbide.
- the phase containing alumina used in the present invention is selected from the group consisting of an alkaline earth metal, a rare earth metal, silicon (Si), titanium (Ti), conoleto (Co), and nickel (Ni). It is preferred to include at least one selected compound. This is because the phase containing alumina (high melting point compound) can be thickened by including these compounds.
- the silicon carbide based porous material of the present invention preferably has an open porosity of 30 to 75% (more preferably 50 to 60%). If the open porosity is less than 30%, the pressure loss increases, and conversely if it exceeds 75%, the strength decreases.
- the silicon carbide based porous material of the present invention preferably has an average pore diameter of 5 to 50 / zm (more preferably 10 to 30 / ⁇ ⁇ ). This is because if the average pore size is less than 5 m, the pressure loss increases, and conversely if it exceeds 50 m, particulate matter leaks.
- the silicon carbide based porous material of the present invention may be used as a structural member (for example, a honeycomb segment) of a honeycomb structure used for, for example, a filter for automobile exhaust gas purification or a catalyst carrier. It can be used suitably.
- the silicon carbide based porous material of the present invention selectively selects only the surface of metallic silicon.
- a phase containing alumina high melting point compound
- a silicon carbide based porous material particles of silicon carbide as an aggregate are bonded together with metal silicon as a binder while maintaining pores between the silicon carbide particles.
- a method for producing a silicon carbide based porous material in which raw materials in which silicon carbide and metal silicon, metal aluminum, or an alloy composed of metal silicon and metal aluminum alloy are mixed are fired in an inert gas atmosphere or a reduced-pressure atmosphere. Then, after producing a metal aluminum monometal silicon monosilicon carbide porous body, the obtained metal aluminum monometal silicon monosilicon carbide porous body is oxidized and fired in an oxygen atmosphere.
- the main feature of the method for producing a silicon carbide based porous material of the present invention is that metal aluminum or an alloy made of metal silicon and metal aluminum is added to silicon carbide and metal silicon which are raw materials. .
- the following effects [A] to [E] can be expected from the method for producing a silicon carbide based porous material of the present invention.
- the silicon carbide based porous body can be coated with a phase containing alumina (a high melting point compound). Since the oxidation reaction of the metallic silicon in the material under the low oxygen partial pressure as shown in the above formula (1) can be reduced, the acid resistance of the silicon carbide based porous material can be improved, and the silicon carbide Since the coating of the phase containing alumina (a compound having a high melting point) can be minimized, the decrease in the porosity of the silicon carbide based porous material can be minimized.
- [D] Metal Aluminum Metal Silicon Carbide Porous Material (Before Oxidizing Treatment) by adding metal aluminum or metal silicon and metal aluminum alloy to the raw material of silicon carbide and metal silicon (Silicon carbide porous body) can be reduced in firing ratio ( size before firing Z dimension after firing).
- the molar ratio of metal aluminum to metal silicon is 0.05 to L5 (more preferably, molar ratio).
- AlZSi is preferably from 0.2 to 0.7). This is because if the molar ratio is less than 0.05, the entire surface of the metal silicon cannot be covered, and conversely if the molar ratio is greater than 1.5, the proportion of silicon carbide bonded to the metallic silicon is reduced, and the heat conduction is reduced. This is because characteristics such as rate are deteriorated.
- the metal aluminum-mu-metal silicon monosilicon carbide porous material obtained after the above-mentioned firing is 700 to 1500 ° C (more preferably) in an oxygen atmosphere. It is preferable to oxidize and bake at 1200 to 1400 ° C. As a result, the obtained silicon carbide based porous material can keep the coated state of the phase containing aluminum (a high melting point compound) on the metal silicon while the silicon carbide is bonded to the metal silicon. Therefore, the acid resistance can be improved.
- the partial pressure of water vapor in the oxygen atmosphere is preferably 10 -5 atm or less, and the partial pressure of oxygen in the oxygen atmosphere is preferably 0.05 atm or more.
- the method for producing a silicon carbide based porous material of the present invention is not less than 700 ° C (more preferably its molar ratio) without lowering the temperature to room temperature after producing the metal aluminum monometal silicon monosilicon carbide porous material.
- the conditions of the oxygen atmosphere are as described above.
- metal aluminum molecular ratio to metal silicon (AlZSi)
- AlZSi metal silicon
- other additives shown in Table 1 or Table 2 80% by mass silicon carbide and 20% by mass metal silicon.
- the obtained metal aluminum monometal silicon monosilicon carbide porous body was oxidized and fired under the atmosphere shown in Table 1 or Table 2.
- the A1 content of the silicon silicon surface and the silicon carbide surface of the obtained silicon carbide based porous material, and the coating state of the phase (high melting point compound) containing alumina on the metal silicon (means: scanning electron microscope Z
- the main A1-containing crystal phase of the phase containing alumina was identified by X-ray diffraction.
- the porosity, average pore diameter, and oxidation resistance of the obtained silicon carbide based porous materials were evaluated. The above results are shown in Tables 1 and 2.
- Each silicon carbide based porous material was measured for average pore diameter by mercury porosimetry, and for porosity by Archimedes method. The evaluation of acid resistance was performed by the following method.
- Tables 1 and 2 show the test temperatures whose appearance changes.
- Examples 1 to 10 show that the surface of metal silicon is selectively covered with a phase containing alumina rather than silicon carbide. In addition to being able to improve, it is possible to minimize the coating of the phase containing alumina (high melting point compound) on silicon carbide, thereby minimizing the porosity of the silicon carbide based porous material. It was out.
- the silicon carbide based porous material of the present invention is a collection filter for exhaust gas, and in particular, a diesel particulate filter (DPF) that collects particulate matter (particulates) in the exhaust gas of diesel engine. It can use suitably at the time of preparation.
- DPF diesel particulate filter
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Products (AREA)
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- Exhaust Gas After Treatment (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Catalysts (AREA)
Description
明 細 書
炭化珪素質多孔体及びその製造方法
技術分野
[0001] 本発明は、自動車排気ガス浄化用のフィルターや触媒担体等に使用される炭化珪 素質多孔体及びその製造方法に関する。
背景技術
[0002] ディーゼルエンジン排気ガスのような含塵流体中に含まれる粒子状物質を捕集除 去するためのフィルター、ある!ヽは排気ガス中の有害物質を浄化する触媒成分を担 持するための触媒担体として、多孔質のハ-カム構造体が広く使用されている。また 、このようなハ-カム構造体の構成材料として、炭化珪素(SiC)粒子のような耐火性 粒子を使用することが知られて ヽる。
[0003] そこで、本願発明者らは、骨材である耐火性粒子 (炭化珪素粒子)と、耐火性粒子 どうしを結合する結合材である金属珪素と、を含む多孔質なハニカム構造体 (Si結合 SiC質多孔体)及びその製造方法を提案した (特許文献 1参照)。この特許文献 1で 開示されたハニカム構造体は、比較的低い焼成温度で歩留まりよく製造出来、熱伝 導率が高ぐ十分に多孔質且つ高比表面積なものであり、フィルタや触媒担体として 好適に利用可能なものである。
[0004] ところが、これら炭化珪素質多孔体に関し、特殊な使用環境や処理方法によっては 、解決すべき課題が残存していることが理解されてきた。
[0005] 例えば、金属珪素を低酸素雰囲気下あるいは還元雰囲気下で加熱すると Siが揮 発したり、下記式(1)のように SiOとして揮発することが知られている。又、これら気体 状態の Siや SiOが酸ィ匕反応等を起こすときには、激しい発熱を伴うことも知られてい る。
Si+ 1/20→SiO†
2
[0006] さらに、発生した SiOガスが雰囲気中の酸素と化合して SiOのファイバーを生成し
2
て表面に析出する。このため、このような酸化反応が生じた部分では、生成した SiO
2 ファイバ一により白色に変色する。
[0007] 上記の問題を解消すベぐ例えば、炭化珪素粒子及び Z又は金属珪素の表面もし くは周囲に酸素を含む相を形成した炭化珪素質多孔体 (特許文献 2参照)が提案さ れているが、特許文献 2に示す炭化珪素質多孔体では、炭化珪素及び Z又は金属 珪素の表面もしくは周囲の酸素を含む相の融点力 高々 1700°Cであり、更にその他 の金属が混入した場合、融点が低下し、耐酸ィ匕性が低下するという問題点があった。
[0008] 上記の問題点を解消するため、前記炭化珪素及び Z又は金属珪素の表面もしくは 周囲の酸素を含む相よりも高い融点を有するアルミナを含む化合物(例えば、コラン ダム)で、炭化珪素及び Z又は金属珪素、特に、金属珪素の表面を被覆することが 検討されてきた。
[0009] 特許文献 1:特開 2002— 201082号公報
特許文献 2:特開 2002— 154882号公報
発明の開示
[0010] 本発明は、上述した従来技術の問題点に鑑みてなされたものであり、その目的とす るところは、金属珪素の表面だけを選択的に高融点の化合物で被覆することにより、 金属珪素の酸化反応が起こる可能性を低減し、耐酸化性を向上させ、且つ、気孔率 の低下を最小限にすることができる炭化珪素質多孔体及びその製造方法を提供す ることにめる。
[0011] 上記目的を達成するため、本発明によって、下記の炭化珪素質多孔体及びその製 造方法が提供される。
[0012] [1] 骨材として炭化珪素の粒子が、金属珪素を結合材として、前記炭化珪素の粒 子相互間に細孔を保持した状態で結合された炭化珪素質多孔体であって、前記炭 化珪素よりも前記金属珪素の表面が選択的にアルミナを含む相で覆われている炭化 珪素質多孔体。
[0013] [2] アルミナを含む相が、アルカリ土類金属、希土類金属、珪素(Si)、チタン (Ti)、 コバルト (Co)、及びニッケル (Ni)力もなる群力も選択される少なくとも 1種以上の化 合物を含む [1]に記載の炭化珪素質多孔体。
[0014] [3] 細孔の開気孔率力 30〜75%である [1]又は [2]に記載の炭化珪素質多孔 体。
[0015] [4] 細孔の平均細孔径カ 5〜50 /ζ πιである [1]〜[3]のいずれかに記載の炭化 珪素質多孔体。
[0016] [5] 体積比熱容量力 2. lJcm_3K_ 1以上である [1]〜[4]のいずれかに記載の炭 化珪素質多孔体。
[0017] [6] [1]〜[5]のいずれかに記載の炭化珪素質多孔体を用いて構成されたノ、二力 ム構造体。
[0018] [7] 骨材として炭化珪素の粒子が、金属珪素を結合材として、前記炭化珪素の粒 子相互間に細孔を保持した状態で結合された炭化珪素質多孔体の製造方法であつ て、炭化珪素及び金属珪素、金属アルミニウムまたは金属珪素と金属アルミニウムか らなる合金を混合した原材料を、不活性ガス雰囲気下又は減圧雰囲気下で焼成して 、金属アルミニウム一金属珪素一炭化珪素多孔体を作製後、得られた金属アルミ二 ゥムー金属珪素一炭化珪素多孔体を、酸素雰囲気下で酸化及び焼成する炭化珪素 質多孔体の製造方法。
[0019] [8] 金属アルミニウムの混合比力 金属珪素に対してモル比(AlZSi)が 0. 05〜1
. 5である [7]に記載の炭化珪素質多孔体の製造方法。
[0020] [9] 原材料を、酸素分圧が 10_4atm以下の不活性ガス雰囲気下又は減圧雰囲気 下で、 600〜1500°Cで焼成する [7]又は [8]に記載の炭化珪素質多孔体の製造方 法。
[0021] [10] 金属アルミニウム一金属珪素一炭化珪素多孔体を、酸素雰囲気下で 700〜1 500°Cで酸化及び焼成する [7]〜 [9]の 、ずれかに記載の炭化珪素質多孔体の製 造方法。
[0022] [11] 金属アルミニウム一金属珪素一炭化珪素多孔体を作製後、室温まで降温す ることなく、 700°C以上の温度で酸素雰囲気へ切り替えて、金属アルミニウム一金属 珪素一炭化珪素多孔体を、前記酸素雰囲気下で 700〜1500°Cで酸化及び焼成す る [7]に記載の炭化珪素質多孔体の製造方法。
[0023] [12] 酸素雰囲気の水蒸気分圧が、 10_5atm以下である [7]〜[11]のいずれかに 記載の炭化珪素質多孔体の製造方法。
[0024] [13] 酸素雰囲気の酸素分圧力 0. 05atm以上である [7]〜 [12]のいずれかに
記載の炭化珪素質多孔体の製造方法。
[0025] 以上説明したように、本発明の炭化珪素質多孔体及びその製造方法は、金属珪素 の表面だけを選択的に高融点の化合物で被覆することにより、金属珪素の酸ィヒ反応 が起こる可能性を低減し、耐酸化性を向上させ、且つ、気孔率の低下を最小限にす ることがでさる。
発明を実施するための最良の形態
[0026] 以下、本発明の炭化珪素質多孔体及びその製造方法を具体的な実施形態に基づ き詳細に説明するが、本発明は、これに限定されて解釈されるもではなぐ本発明の 範囲を逸脱しない限りにおいて、当業者の知識に基づいて、種々の変更、修正、改 良をカ卩ぇ得るものである。
[0027] 本発明に係る炭化珪素質多孔体は、骨材として炭化珪素の粒子が、金属珪素を結 合材として、炭化珪素の粒子相互間に細孔を保持した状態で結合された炭化珪素 質多孔体であって、炭化珪素よりも金属珪素の表面が選択的にアルミナを含む相で 覆われているものである。
[0028] ここで、本発明で用いるアルミナを含む相は、アルカリ土類金属、希土類金属、珪 素(Si)、チタン (Ti)、コノ レト (Co)、及びニッケル (Ni)からなる群から選択される少 なくとも 1種以上の化合物を含むことが好ましい。これは、これらの化合物を含むこと により、アルミナを含む相(高融点の化合物)を厚くすることができるためである。
[0029] また、本発明の炭化珪素質多孔体は、細孔の開気孔率が 30〜75% (より好ましく は、 50〜60%)であることが好ましい。開気孔率が 30%より小さいと圧力損失が大き くなり、逆に 75%を超えて大きいと強度が低下する。
[0030] 更に、本発明の炭化珪素質多孔体は、細孔の平均細孔径が、 5〜50 /z m (より好ま しくは、 10〜30 /ζ πι)あることが好ましい。平均細孔径が 5 mより小さいと圧力損失 が大きくなり、逆に 50 mより大きいと粒子状物質が漏出するためである。
[0031] 尚、本発明の炭化珪素質多孔体は、例えば、自動車排気ガス浄ィ匕用のフィルタや 触媒担体等に使用されるハニカム構造体の構成部材 (例えば、ハニカムセグメント)と しても好適に用いることができる。
[0032] 以上のことから、本発明の炭化珪素質多孔体は、金属珪素の表面だけを選択的に
アルミナを含む相(高融点の化合物)で被覆することにより、金属珪素の酸化反応が 起こる可能性を低減し、耐酸化性を向上させ、且つ、気孔率の低下を最小限にする ことができる。
[0033] 次に、本発明の炭化珪素質多孔体の製造方法について説明する。
[0034] 本発明に係る炭化珪素質多孔体の製造方法は、骨材として炭化珪素の粒子が、金 属珪素を結合材として、炭化珪素の粒子相互間に細孔を保持した状態で結合された 炭化珪素質多孔体の製造方法であって、炭化珪素及び金属珪素、金属アルミニウム または金属珪素と金属アルミニウムカゝらなる合金を混合した原材料を、不活性ガス雰 囲気下又は減圧雰囲気下で焼成して、金属アルミニウム一金属珪素一炭化珪素多 孔体を作製後、得られた金属アルミニウム一金属珪素一炭化珪素多孔体を、酸素雰 囲気下で酸ィ匕及び焼成するものである。
[0035] 本発明の炭化珪素質多孔体の製造方法の主な特徴は、原材料である炭化珪素及 び金属珪素に、金属アルミニウム、または、金属珪素と金属アルミニウム力 なる合金 を添加することにある。これにより、本発明の炭化珪素質多孔体の製造方法は、以下 に示す [A]〜 [E]の効果が期待できる。
[0036] [A]金属珪素の表面だけを選択的にアルミナを含む相(高融点の化合物)で被覆 することができるため、アルミナを含む相(高融点の化合物)で、炭化珪素質多孔体 中の金属珪素の上記式(1)に示すような低酸素分圧下における酸化反応を低減す ることができるため、炭化珪素質多孔体の耐酸ィ匕性を向上することができるとともに、 炭化珪素へのアルミナを含む相(高融点の化合物)の被覆を最小限にすることができ るため、炭化珪素質多孔体の気孔率の低下を最小限にすることができる。
[0037] [B]炭化珪素及び金属珪素の表面にある酸化珪素を下記式 (2)に従って除去する ことで、炭化珪素に対する金属珪素の濡れ性を向上させることができる。
3SiO +4Al→3Si+ 2Al O - -- (2)
2 2 3
[0038] [C]炭化珪素及び金属珪素の原材料に、金属アルミニウム、または、金属珪素と金 属アルミニウム力 なる合金を添加することにより、結合部の融点が低下するため、金 属アルミニウム一金属珪素一炭化珪素多孔体 (酸化処理前の炭化珪素質多孔体)の 焼成温度を低くすることができるため、経済的である。
[0039] [D]炭化珪素及び金属珪素の原材料に、金属アルミニウム、または、金属珪素と金 属アルミニウム力 なる合金を添加することにより、金属アルミニウム 金属珪素 炭 化珪素多孔体 (酸ィ匕処理前の炭化珪素質多孔体)の焼成割り掛け(=焼成前寸法 Z 焼成後寸法)を小さくさせることができる。
[0040] [E]体積比熱容量の小さ!/、金属珪素の表面を高体積比熱容量の化合物であるァ ルミナを含む相で被覆することができるため、高温のガスに曝された炭化珪素多孔体 中の金属珪素の温度上昇を抑制することができるため、炭化珪素質多孔体の温度上 昇を抑制することができる。
[0041] ここで、本発明の炭化珪素質多孔体の製造方法は、金属アルミニウムの混合比力 金属珪素に対してモル比 (AlZSi)が 0. 05〜: L 5 (より好ましくは、モル比 (AlZSi) が 0. 2〜0. 7)であることが好ましい。これは、モル比が 0. 05より小さいと金属珪素 の表面を全て覆うことができなくなり、逆にモル比が 1. 5より大きいと炭化珪素を金属 珪素で結合する割合が小さくなり、熱伝導率などの特性が低下するためである。
[0042] また、本発明の炭化珪素質多孔体の製造方法は、原材料を、酸素分圧が 10_4at m以下の不活性ガス雰囲気下又は減圧雰囲気下で、 600〜1500°C (より好ましくは 、そのモル比 (AlZSi)に対する初晶温度)で金属アルミニウム一金属珪素一炭化珪 素多孔体を焼成することが好まし ヽ。
[0043] 更に、本発明の炭化珪素質多孔体の製造方法は、上記焼成後に得られた金属ァ ルミ-ゥムー金属珪素一炭化珪素多孔体を、酸素雰囲気下で 700〜1500°C (より好 ましくは、 1200〜1400°C)で酸ィ匕及び焼成することが好ましい。これにより、得られ た炭化珪素質多孔体は、炭化珪素が金属珪素と結合されているとともに、金属珪素 へのアルミナを含む相(高融点の化合物)の被覆状態を良好に保持することができる ため、耐酸ィ匕性を向上させることができる。
[0044] 尚、上記酸素雰囲気の水蒸気分圧は、 10_5atm以下であり、酸素雰囲気の酸素 分圧が、 0. 05atm以上であることが好ましい。
[0045] 更に、本発明の炭化珪素質多孔体の製造方法は、金属アルミニウム一金属珪素一 炭化珪素多孔体を作製後、室温まで降温することなぐ 700°C以上 (より好ましくは、 そのモル比 (AlZSi)に対する初晶温度)の温度で酸素雰囲気へ切り替えて、金属
アルミニウム 金属珪素 炭化珪素多孔体を、酸素雰囲気下で 700〜 1500°C (より 好ましくは、 1200〜1400°C)で酸ィ匕及び焼成することがより好ましい。尚、上記酸素 雰囲気の条件は、上述の通りである。
実施例
[0046] 以下、本発明を実施例によって更に具体的に説明するが、本発明は、これらの実 施例によって 、かなる制限を受けるものではな 、。
[0047] (実施例 1〜10、比較例 1〜9)
80質量%の炭化珪素及び 20質量%の金属珪素に、表 1又は表 2に示す金属アル ミニゥム (金属珪素に対するモル比 (AlZSi) )及びその他添加物を添加 ·混合した原 材料を、表 1又は表 2に示す雰囲気下で、表 1又は表 2に示す条件で焼成して、金属 アルミニウム一金属珪素一炭化珪素多孔体を作製した。得られた金属アルミニウム 一金属珪素一炭化珪素多孔体を、表 1又は表 2に示す雰囲気下で酸ィ匕及び焼成し た。それぞれ得られた炭化珪素質多孔体の金属珪素表面及び炭化珪素表面の A1 含有量、および、金属珪素へのアルミナを含む相(高融点の化合物)の被覆状態を( 手段:走査型電子顕微鏡 Zエネルギー分散型 X線分析装置)で測定'評価するととも に、アルミナを含む相の主な A1含有結晶相の同定を X線回折法で行った。更に、そ れぞれ得られた炭化珪素質多孔体の気孔率、平均細孔径及び耐酸化性の評価を 行った。以上の結果を表 1及び表 2に示す。尚、それぞれの炭化珪素質多孔体は、 水銀圧入法にて平均細孔径を測定し、アルキメデス法により気孔率を測定した。尚、 耐酸ィ匕性の評価は、以下の方法によって実施された。
[0048] (耐酸化性の評価)
「耐酸ィ匕性」の評価は低酸素分圧下の酸ィ匕試験によって行った。すなわち、得られ た炭化珪素質多孔体を、電気炉内で酸素分圧が 0. Olatmの Arガス雰囲気下で試 験温度、 10分間保持し、その外観変化を検査した。上記式(1)によって生成した Si Oガスがさらに雰囲気中の酸素とィ匕合して SiOとなった際には、外観が白く変化する
2
。その外観変化する試験温度を表 1及び表 2に示す。
〔s〔005
[0051] (考察:実施例 1〜: LO、比較例 1〜9)
表 1及び表 2の結果から、実施例 1〜10は、炭化珪素よりも金属珪素の表面が選択 的にアルミナを含む相で覆われているため、炭化珪素質多孔体の耐酸ィ匕性を向上 することができるとともに、炭化珪素へのアルミナを含む相(高融点の化合物)の被覆 を最小限にすることができるため、炭化珪素質多孔体の気孔率の低下を最小限にす ることがでさた。
[0052] 比較例 1〜3及び比較例 8では、金属珪素の表面がアルミナを含む相で覆われて いない、もしくは、覆われる表面が少ないため、得られた炭化珪素質多孔体の耐酸化 性が不十分であった。
[0053] 一方、比較例 4では、炭化珪素よりも金属珪素の表面が選択的にアルミナを含む相 で覆われていないため、金属珪素だけでなぐ炭化珪素も同様に被覆されてしまうた め、得られた炭化珪素質多孔体の気孔率が低下することを確認した。
[0054] また、比較例 5、比較例 6及び比較例 9では、炭化珪素が金属珪素と結合されて!、 ないため、炭化珪素質多孔体として形成されな力つた。
[0055] 比較例 7では、金属アルミニウムが酸ィ匕しな 、ため、得られた炭化珪素質多孔体の 耐酸化性が不十分であった。
産業上の利用可能性
[0056] 本発明の炭化珪素質多孔体は、排ガス用の捕集フィルタ、中でも、ディーゼルェン ジンの排ガス中の粒子状物質 (パティキュレート)等を捕集するディーゼルパティキュ レートフィルタ (DPF)の作製時に好適に用いることができる。
Claims
[1] 骨材として炭化珪素の粒子が、金属珪素を結合材として、前記炭化珪素の粒子相 互間に細孔を保持した状態で結合された炭化珪素質多孔体であって、前記炭化珪 素よりも前記金属珪素の表面が選択的にアルミナを含む相で覆われている炭化珪素 質多孔体。
[2] 前記アルミナを含む相力 アルカリ土類金属、希土類金属、珪素(Si)、チタン (Ti) 、コバルト(Co)、及びニッケル (Ni)力もなる群力も選択される少なくとも 1種以上の化 合物を含む請求項 1に記載の炭化珪素質多孔体。
[3] 前記細孔の開気孔率が、 30〜75%である請求項 1又は 2に記載の炭化珪素質多 孔体。
[4] 前記細孔の平均細孔径が、 5〜50 111でぁる請求項1〜3のぃずれか1項に記載 の炭化珪素質多孔体。
[5] 体積比熱容量が、 2. lJcm_3K_1以上である請求項 1〜4のいずれか 1項に記載の 炭化珪素質多孔体。
[6] 請求項 1〜5のいずれか 1項に記載の炭化珪素質多孔体を用いて構成されたノ、二 カム構造体。
[7] 骨材として炭化珪素の粒子が、金属珪素を結合材として、前記炭化珪素の粒子相 互間に細孔を保持した状態で結合された炭化珪素質多孔体の製造方法であって、 炭化珪素及び金属珪素、金属アルミニウムまたは金属珪素と金属アルミニウム力 な る合金を混合した原材料を、不活性ガス雰囲気下又は減圧雰囲気下で焼成して、金 属アルミニウム一金属珪素一炭化珪素多孔体を作製後、得られた金属アルミニウム 一金属珪素一炭化珪素多孔体を、酸素雰囲気下で酸化及び焼成する炭化珪素質 多孔体の製造方法。
[8] 前記金属アルミニウムの混合比力 前記金属珪素に対してモル比 (AlZSi)が 0. 0 5〜1. 5である請求項 7に記載の炭化珪素質多孔体の製造方法。
[9] 前記原材料を、酸素分圧が 10_4atm以下の不活性ガス雰囲気下又は減圧雰囲気 下で、 600〜 1500°Cで焼成する請求項 7又は 8に記載の炭化珪素質多孔体の製造 方法。
[10] 前記金属アルミニウム一金属珪素一炭化珪素多孔体を、酸素雰囲気下で 700〜1 500°Cで酸化及び焼成する請求項 7〜9のいずれか 1項に記載の炭化珪素質多孔 体の製造方法。
[11] 前記金属アルミニウム一金属珪素一炭化珪素多孔体を作製後、室温まで降温する ことなぐ 700°C以上の温度で酸素雰囲気へ切り替えて、前記金属アルミニウム一金 属珪素一炭化珪素多孔体を、前記酸素雰囲気下で 700〜1500°Cで酸化及び焼成 する請求項 7に記載の炭化珪素質多孔体の製造方法。
[12] 前記酸素雰囲気の水蒸気分圧が、 10_5atm以下である請求項 7〜11のいずれか 1項に記載の炭化珪素質多孔体の製造方法。
[13] 前記酸素雰囲気の酸素分圧が、 0. 05atm以上である請求項 7〜12のいずれか 1 項に記載の炭化珪素質多孔体の製造方法。
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JP2019167279A (ja) * | 2018-03-26 | 2019-10-03 | 日本碍子株式会社 | 多孔質材料、セル構造体および多孔質材料の製造方法 |
JP7025969B2 (ja) | 2018-03-26 | 2022-02-25 | 日本碍子株式会社 | 多孔質材料、セル構造体および多孔質材料の製造方法 |
JP2021526961A (ja) * | 2018-06-06 | 2021-10-11 | ネクスセリス イノベーション ホールディングス, エルエルシーNexceris Innovation Holdings, Llc | 触媒支持材料、触媒支持体、触媒及び触媒を用いた反応方法 |
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US20090011179A1 (en) | 2009-01-08 |
EP2006269A4 (en) | 2013-01-16 |
EP2006269A9 (en) | 2009-07-08 |
JP5180821B2 (ja) | 2013-04-10 |
KR20080105152A (ko) | 2008-12-03 |
EP2006269A2 (en) | 2008-12-24 |
US8029882B2 (en) | 2011-10-04 |
JPWO2007119287A1 (ja) | 2009-08-27 |
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