TW202334382A - 耐火製品及其用途 - Google Patents
耐火製品及其用途 Download PDFInfo
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- TW202334382A TW202334382A TW111145081A TW111145081A TW202334382A TW 202334382 A TW202334382 A TW 202334382A TW 111145081 A TW111145081 A TW 111145081A TW 111145081 A TW111145081 A TW 111145081A TW 202334382 A TW202334382 A TW 202334382A
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- 239000000203 mixture Substances 0.000 claims abstract description 35
- 239000011159 matrix material Substances 0.000 claims abstract description 23
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 15
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000004048 modification Effects 0.000 claims abstract description 4
- 238000012986 modification Methods 0.000 claims abstract description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 42
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 20
- 239000010431 corundum Substances 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 238000010304 firing Methods 0.000 claims description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical group [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 claims description 4
- 239000011819 refractory material Substances 0.000 claims description 4
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 3
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 22
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 2
- 229910009474 Y2O3—ZrO2 Inorganic materials 0.000 abstract 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 21
- 239000011449 brick Substances 0.000 description 19
- 239000000047 product Substances 0.000 description 18
- 239000000843 powder Substances 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 8
- 230000004580 weight loss Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910002090 carbon oxide Inorganic materials 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000010987 cubic zirconia Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000012106 screening analysis Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229920001732 Lignosulfonate Polymers 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011451 fired brick Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 230000002028 premature Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 229910052572 stoneware Inorganic materials 0.000 description 2
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910002078 fully stabilized zirconia Inorganic materials 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009993 protective function Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000011214 refractory ceramic Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000003826 uniaxial pressing Methods 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
一種成型及燒製的粗陶瓷耐火製品以及一種製備該製品之方法及該製品的用途,該成型及燒製的粗陶瓷耐火製品包含
(a) 化學組成物,其包含以下含量:Al
2O
3:至少40 wt.%;Y
2O
3: 2.0-57 wt.%;ZrO
2:低於42.0 wt.%;及
(b) 黏結基質,其至少包含具有三元系統Al
2O
3-Y
2O
3-ZrO
2立方改性的含氧化釔的結晶混合氧化物。
Description
本發明關於含有Al
2O
3低SiO
2的粗陶瓷燒製耐火製品,其製備方法及該製品的用途,該製品的黏結基質至少包含具有三元系統Al
2O
3-Y
2O
3-ZrO
2立方改性的結晶性含氧化釔之混合氧化物相。
就本發明的意義上,用語「含有Al
2O
3」意指Al
2O
3含量至少40.0 wt. %。
眾所皆知,粗陶瓷製品係基於晶粒尺寸達6 mm且在特殊情況下達25 mm的原料。這些燒製製品的三個主要結構成分是支架(scaffolding)晶粒、黏結基質及孔隙(pores) (參考G. Routschka and H. Wuthnow, “Handbook of Refractory Materials”, chapter 2, ISBN 978-3-8027-3162-4)。與粗陶瓷製品不同,精密陶瓷製品的結構根據定義呈現小於0.2 mm的晶粒(肉眼看來是均質的)。
EP 0309091 B1敘述耐火陶瓷材料,其由氧化釔粉末及氧化鋁粉末的混合物(含有至少70 mole %氧化釔及11至30 mole %氧化鋁)形成且主要由單斜晶系釔鋁氧化物(Y
4Al
2O
9, YAM)組成。具有5.3至16.2 wt. % Al
2O
3的精密陶瓷不透明材料的特徵為沒有開放型孔隙(open pores)的結構且表現對熔融稀土-鐵合金的抵抗性(resistance)。建議將等靜壓壓製材料(isostatically pressed material)用作鑄造熔融金屬的噴嘴。
包含氧化鋁及氧化釔穩定的四方晶氧化鋯以及如果適用的話還有額外的單斜晶系氧化鋯的精密陶瓷材料在工程應用中被稱為氧化鋯增韌氧化鋁(ZTA) (例如US 4,960,441及EP 0300716 B1)。精密氧化鋯顆粒 (典型為10-20 wt. %)均勻分散在µ-尺寸的氧化鋁基體中,從而形成比單獨氧化鋁更抗斷裂的微觀結構。當處於應力下,介穩態四方晶氧化鋯會轉變為單斜晶系相,這會在體積膨脹的情況下發生,從而產生各種增韌機制。
對於工作溫度高於1000°C且含有氫氣(H
2)及一氧化碳(CO)的襯裡燃燒室或熔爐,使用在礦物學上主要由α-Al
2O
3(剛玉)組成並表現必要的低二氧化矽和鐵含量的粗陶瓷耐火氧化鋁材料是眾所周知的。眾所皆知,SiO
2及Fe
2O
3在這些還原條件下都不穩定。因此,製造這些不含氧化釔的材料的原料基礎是高純度粒狀合成熔融及/或燒結剛玉以及粉狀煅燒氧化鋁。
市場上可提供的化學高純度和直接覆高燒製剛玉磚 (> 98 wt. % Al
2O
3)的特徵是具有高耐熱性和高溫負載下使用所需的穩定性,其係根據作為負載下的耐火度(refractoriness)和壓縮潛變的標準量測。例如,這些粗陶瓷材料作為用於製造合成氣的反應器壓力容器的襯裡(「熱面」)的典型應用就是基於此。然而,當在高溫下存在含有碳氧化物、氫氣、特別是至少暫時存在蒸汽的還原氣氛時,磚表面的氧化鋁被化學還原為氣態次氧化鋁(aluminium sub-oxides)及/或氫氧化鋁,由此已知磚的氧化鋁黏結基質優先受到攻擊。這種氧化鋁揮發的特徵是隨溫度升高到1100°C以上呈指數增長,最高熱面溫度可達1550°C。熱面的典型溫度將在1200-1400°C的範圍內。因此,最嚴重的揮發腐蝕效應發生在反應器容器的上部(upper part),可以直接量測為剛玉材料的厚度損失或重量損失。結果,氣態含鋁製品遷移到反應器的較冷區域及/或下游製程設備中的較冷表面。在此,它們沉澱為氧化鋁並形成沉積物,已知會引起各種嚴重的問題。特別是,使用固定催化劑床操作的反應器內的沉積物會因流動路徑堵塞而導致代價高昂的過早停機。此外,通過耐火襯裡的熱氣體旁路會導致過熱,可能威脅壓力容器的安全操作並導致大規模的維修。
美國專利申請公開號2019/0218151建議一種氧化釔穩定的立方氧化鋯耐火磚材料,該材料在含有蒸汽的還原熱氣體氣氛中表現高耐化性。粗陶瓷材料的Al
2O
3含量僅限於0.05-6 wt. %以避免在應用過程過早磨損,從而少量的Al
2O
3應該有利地促進介穩態四方晶ZrO
2的形成。然而,眾所皆知,此種氧化鋯材料遠比剛玉磚貴。也不能排除立方氧化鋯相在使用過程至少部分不穩定,伴隨著與溫度相關的體積變化,可能導致臨界裂紋的形成。因此,將這些高密度材料作為內磚襯裡材料的商業用途不是可行的選項。
本發明的主要目的是提供一種含有Al
2O
3的成型及燒製的粗陶瓷耐火製品,該製品在高溫下表現對含有蒸汽的還原熱氣體的高抵抗性和高抗潛變性。
本發明另一目的是提供一種製造該製品的方法及該製品的特別用途。
本發明係基於以下令人驚訝的認知:當燒製製品的黏結基質至少包含具有三元系統Al
2O
3-Y
2O
3-ZrO
2立方改性的含氧化釔的結晶混合氧化物,含有Al
2O
3的粗陶瓷耐火製品對還原含蒸汽的熱氣體的抵抗性可以提高到顯著的可測量效應。已發現,根據本發明的耐火製品的黏結基質既對耐火製品發揮有效的保護功能以防止氧化鋁蒸發,又有利地有助於耐火製品的高耐熱性和穩定性。
根據本發明,提供的燒製粗陶瓷耐火製品包含以下特徵:
- 製品具有的化學組成分別為根據以下數量的以下氧化物:
Al
2O
3:至少40.0 wt.%;Y
2O
3:2.0-57.0 wt.%;ZrO
2:低於42.0 wt.%;
- 製品的黏結基質至少包含具有三元系統Al
2O
3-Y
2O
3-ZrO
2立方改性的含氧化釔的結晶混合氧化物。
為了本發明的目的,具有立方晶體結構的含氧化釔之混合氧化物為耐火釔鋁石榴石(Y
3Al
5O
12, YAG)或耐火氧化釔完全穩定的氧化鋯(Y-FSZ)或兩者的混合物。化學組成為42.9 wt. % Al
2O
3和57.1 wt.% Y
2O
3的YAG是二元系統Y
2O
3-Al
2O
3中最富含Al
2O
3的化合物。YAG具有約1900°C的高熔化溫度和與Al
2O
3類似的熱膨脹係數。Y-FSZ含有約8 mol. % (約13 wt. %)Y
2O
3並在約2680°C熔化。
作為黏結基質的至少部分組分的YAG和Y-FSZ可藉由X射線粉末繞射分析在成品耐火製品上檢測到,例如使用Rietveld方法及/或顯微鏡檢查例如薄片,如果需要還包括製品的確定化學組成,例如根據DIN EN ISO 12677量測。
根據本發明,已發現除了氧化物Al
2O
3, Y
2O
3和ZrO
2之外,還存在可以存在於根據本發明的耐火製品中的其它氧化物(例如作為原料雜質),可能對含蒸汽的還原熱氣體的抵抗性及/或熱性質產生負面影響。這些氧化物包括,例如SiO
2、TiO
2、Fe
2O
3和鹼,其在成品中的總含量不應超過1.5 wt.%,較佳不應超過1.0 wt.%。此外,應考慮到HfO
2出現在由鋯石砂合成的ZrO
2中(例如通過電熔),含量高達2 wt.%。在這方面,在一個較佳的具體實例中,根據本發明的耐火製品包含這樣的化學組成,根據該化學組成,氧化物SiO
2、TiO
2、Fe
2O
3、鹼和HfO
2的總和最多2.2 wt.%,較佳最多1.7 wt.%,例如由DIN EN ISO 12677確定。
因此,作為用於提供根據本發明的製品的支架晶粒的原料,較佳使用顆粒狀高純度熔融剛玉及/或燒結剛玉,其具有> 98.5 wt. %、較佳 > 99 wt. %、最佳 > 99.5 wt. %的Al
2O
3含量且具有粗陶瓷製品常用的晶粒尺寸,例如0-1 mm及/或1-5 mm。晶粒尺寸藉由篩選分析,例如根據DIN 66165而確定。根據某些非限制具體實例,其他具有前述晶粒尺寸的含有Al
2O
3顆粒狀原料例如燒結及/或熔融尖晶石及/或燒結及/或熔融YAG及/或系統Al
2O
3-Y
2O
3-ZrO
2的燒結及/或熔融材料,也可至少部分地提供用於耐火製品的支架晶粒。
本發明還涵蓋製造耐火製品的方法,包括提供黏結基質的步驟,該黏結基質至少包含具有三元系統Al
2O
3-Y
2O
3-ZrO
2立方改性的含氧化釔的結晶混合氧化物。
根據某些非限制具體實例,YAG可被提供在耐火製品的黏結基質中,例如在耐火製品於1500°C至1800°C、較佳1600°C至1760°C溫度範圍內燒製期間,經由Al
2O
3和Y
2O
3以適當的混合比以原位反應而提供。生成YAG的反應經由Y
4Al
2O
9(YAM,單斜晶系)和YAlO
3(YAP,斜方晶系)的中間體形成而進行。在本發明的全文中,原位形成的YAG在較低溫度例如1400°C燒製時已經被檢測到。然而,已發現當根據本發明的製品在上述更高的燒製溫度燒製時,提供足夠高的耐熱性和穩定性。
氧化釔原料可以具有高純度的合成製品形式在市場上獲得,其中在本發明的意義上,純度是指Y
2O
3含量/稀土氧化物總量的比例(Y
2O
3/TREO)。Y
2O
3具有立方結構,熔點約為2410°C。根據本發明,使用例如純度>98.5%、較佳≥99%、最佳≥99.9%的氧化釔粉末,其中非稀土雜質例如Fe、Al、Ca、SO
4 2-和Cl
-的總含量低於0.15 wt.%。所用氧化釔粉末的平均晶粒尺寸小於63 μm,較佳小於25 μm,更佳小於10 μm,例如小於10 μm,例如藉由雷射繞射量測(d
50-值)。
作為形成YAG的Al
2O
3原料,較佳使用在市場上獲得的高純度熔融氧化鋁(熔融剛玉)及/或燒結氧化鋁(燒結剛玉)及/或研磨煅燒氧化鋁粉末,其特徵在於Al
2O
3含量 > 99 wt. %,特別是> 99.5 wt. %。由此,在本發明的全文中,已發現可以提供Al
2O
3原料作為晶粒尺寸小於0.5 mm,較佳小於0.1 mm的粉末及/或具有通常用於粗陶瓷製品的晶粒尺寸的晶粒,例如0-1 mm及/或1-5 mm,其中晶粒尺寸由篩選分析確定,例如根據DIN 66165。令人驚訝地發現,在成型耐火製品的燒製期間,氧化釔甚至藉由形成YAG作為黏結基質的一部分而在其表面與較粗的剛玉晶粒發生反應。
根據某些非限制實施方案,Y-FSZ可以在耐火製品的黏結基質中獲得,其係經由耐火製品在1500°C至1800°C、較佳1650°C至1760°C的溫度範圍內燒製期間,較佳經由市售單斜晶系及/或四方晶ZrO
2及Y
2O
3粉末以適當混合物的原位反應而獲得,ZrO
2較佳以粉末形式提供,晶粒尺寸小於0.5 mm,較佳小於0.1 mm,例如以篩選通道(sieve passage)確定。
根據某些非限制實施方案,YAG和Y-FSZ的混合物可被提供在耐火製品的黏結基質中,其係使用如上所述的原料,在耐火製品於1500°C至1800°C、較佳1650°C至1760°C溫度範圍內燒製期間,經由Al
2O
3、Y
2O
3和ZrO
2以適當的混合比以原位反應而提供。在本文中,確認了形成YAG只在形成Y-FSZ完成之後發生。
在本發明的全文中,發現分別製備的(合成的)YAG,例如藉由固態反應,或分別合成製備的Y-FSZ,例如市售的電熔融,或二者的混合物,當用作原料時,可以至少按比例提供在耐火製品的黏結基質中,該原料較佳為晶粒尺寸小於0.5 mm,較佳小於0.1 mm的粉末形式,例如以篩選通道確定。
根據某些非限制具體實例,YAG可分別製備,例如藉由以合適的比例混合上述類型的氧化釔及氧化鋁粉末,例如以化學計量,加入合適的有機壓製劑及/或黏合劑諸如木質素磺酸鹽或蠟乳液,視需要的與水組合,從而形成可壓製(pressable)組成物。接著進行成型製程,例如單軸壓製或擠壓,隨後在高於1400 °C,較佳高於1450 °C的溫度燒製成型和乾燥的物體。以在壓碎和篩選以及視需要的研磨之後可以獲得所欲最大晶粒尺寸的方式選擇燒製成型物體的尺寸。
根據本發明另一態樣,當用作具有粗陶瓷製品常見晶粒尺寸(例如0.1-1 mm及/或1-5 mm,例如藉由篩選分析確定)的原料,分別製備的YAG可以至少部分地作為含有Al
2O
3的支架晶粒提供。
根據本發明,具有上述晶粒尺寸的含有Al
2O
3的支架晶粒與YAG及/或Y-FSZ形成組分(分別具有粉狀YAG及/或Y-FSZ)的混合物、及暫時黏合劑或黏合劑混合物(例如有機黏合劑諸如木質素磺酸鹽及糊精)以及若需要時與水混合。暫時黏合劑及水可以必要的比例添加,特別是使製備的批料(混合物)具有潮濕易碎一致性(moist crumbly consistency)的比例。粗陶瓷混合物經成型為磚。對成型而言,可以使用各種眾所皆知的製程,從而特別是必須考慮所欲幾何形狀的複雜性和要成型的件數(「Handbook of Refractory Materials」,同上)。在適用的情況下,成型製品仍可在燒製前乾燥,例如在乾燥器中乾燥。隨後在1500°C至1800°C、較佳1650°C至1760°C的溫度範圍內燒製磚。較佳在上述燒製溫度燒製進行4至12小時範圍內的持續時間。
根據本發明的製品較佳用於熔爐、重組器諸如二次蒸汽重組器、反應器或具有還原氣氛的容器。在這方面,本發明的另一個目的是使用根據本發明的製品作為氣化裝置的襯裡材料,特別是作為用於在高於1000°C的溫度製備富含氫氣和一氧化碳的合成氣的容器的襯裡材料。
本發明的另一個目的是提供一種用於在高於1000°C的溫度製備富含氫氣和一氧化碳的合成氣的容器,該容器至少部分以根據本發明的製品為襯裡,例如作為牆磚及/或作為燃燒區和催化區之間的隔板。
歸納起來,本發明的特徵為:
1. 一種成型及燒製的粗陶瓷耐火製品,其包含
(a) 化學組成物,其包含以下含量:Al
2O
3:至少40 wt.%;Y
2O
3: 2.0-57 wt.%;ZrO
2:低於42.0 wt.%;及
(b) 黏結基質,其至少包含具有三元系統Al
2O
3-Y
2O
3-ZrO
2立方改性的含氧化釔的結晶混合氧化物。
2. 如特徵1之耐火製品,其中具有三元系統的立方晶體結構的該含氧化釔的結晶混合氧化物係釔鋁石榴石(Y
3Al
5O
12)。
3. 如特徵1之耐火製品,其中具有立方晶體結構的該含氧化釔的結晶混合氧化物係氧化釔完全穩定的氧化鋯,或氧化釔完全穩定的氧化鋯及Y
3Al
5O
12的混合物。
4. 如特徵1至3中任一項之耐火製品,其中該製品中進一步含有的氧化物SiO
2、TiO
2、Fe
2O
3、鹼和HfO
2的總和最多2.2 wt.%,較佳最多1.7 wt.%。
5. 如特徵1至4中任一項之耐火製品,其中該化學組成物包含至少60 wt. %的Al
2O
3。
6. 如特徵1至5中任一項之耐火製品,其中該化學組成物包含2.0至25 wt. %之間的Y
2O
3
7. 一種製備成型及燒製的粗陶瓷耐火物之方法,該粗陶瓷耐火物包含化學組成物,該化學組成物包含以下含量:Al
2O
3:至少40 wt.%;Y
2O
3:2.0-57 wt.%;ZrO
2:低於42.0 wt.%,該方法包含以下步驟:
提供黏結基質,其至少包含具有三元系統Al
2O
3-Y
2O
3-ZrO
2立方改性的含氧化釔的結晶混合氧化物。
8. 如特徵7之方法,其中用於提供該含氧化釔的結晶混合氧化物的Y
2O
3的純度係Y
2O
3/稀土氧化物總量,該純度>98.5%,諸如>99%或諸如99.9%。
9. 如特徵7或8之方法,其中原料混合物包含顆粒狀高純度熔融剛玉及/或燒結剛玉,其具有> 98.5 wt. %、較佳 > 99 wt. %、最佳 > 99.5 wt. %的Al
2O
3含量且具有0-1 mm之間及/或1-5 mm之間的晶粒尺寸。
10. 如特徵7至9中任一項之方法,其中該黏結基質係在該原料混合物成型後燒製該原料混合物而形成。
11. 如特徵7至10中任一項之方法,其中該Y
2O
3的平均晶粒尺寸小於63 µm,諸如小於25 µm或諸如小於10 µm。
12. 一種如特徵1至6中任一項之製品之用途,其係作為暴露於還原氣氛的耐火材料。
13. 一種用於製備富含氫氣和一氧化碳的氣體的容器,該容器包含特徵1至6中任一項之製品。
以下實施例及圖示僅供說明之用,並不構成對本發明保護範圍的限制。
實施例
表1列出用於製備例示和傳統比較氧化鋁磚(參考)的粉末狀和顆粒狀原料的含量。所用氧化釔粉末的平均晶粒尺寸(d
50)約為5 µm,純度(Y
2O
3/TREO)為99.99 %。在強力混合器中完成成分與額外的約0.8 wt. %木質素磺酸鹽和約2.2 wt.%水的均勻混合。將以這種方式獲得的潮濕易碎混合物在約80 MPa的成型壓力下壓制,得到體積約4300 cm
3(磚高度約15 cm)的磚。在約110°C乾燥至恆重後,將乾燥的磚在1720°C的溫度燒製6小時。
燒製磚的某些性質如表1所示。YAG和Y-FSZ的含量藉由包括化學分析的X射線粉末繞射分析確定。根據DIN EN 993-1量測體積密度和表觀孔隙度,根據DIN EN 993-5量測冷抗碎強度,並根據DIN EN 993-9壓縮潛變作為耐熱性和穩定性的量測。
表1
項目 | 實施例 | 1 | 2 | 3 | 4 | 5 | 6 | 參考 |
混合物(wt. %) | 熔融氧化鋁 1-3 mm 熔融氧化鋁 0-1 mm 煅燒氧化鋁 0-0.1 mm 氧化釔 0-0.1 mm 單斜晶系 ZrO 20-0.1 mm Y-FSZ 0-0.1 mm | 45 40 6.4 8.6 --- --- | 45 40 3.3 11.8 --- --- | 45 40 --- 15 --- --- | 45 40 --- 5.8 9.2 --- | 45 40 --- 2.1 12.9 --- | 42.5 27.5 --- --- --- 30 | 45 40 15 --- --- --- |
性質 | YAG (wt. %) Y-FSZ (wt. %) | 15.1 --- | 20.7 --- | 26.3 --- | 7.7 10.6 | --- 15 | --- 30 | --- --- |
Al 2O 3(wt. %) Y 2O 3(wt. %) ZrO 2(wt. %) | 90.9 8.6 --- | 87.7 11.8 --- | 84.5 15.0 --- | 84.5 5.8 8.9 | 84.5 2.1 12.4 | 69.9 3.9 25.1 | 99.5 --- --- | |
∑SiO 2, TiO 2, Fe 2O 3, 鹼, HfO 2(wt. %) | 0.4 | 0.3 | 0.3 | 0.7 | 0.8 | 0.9 | 0.4 | |
體積密度(g/cm³) | 3.26 | 3.25 | 3.24 | 3.30 | 3.28 | 3.40 | 3.24 | |
表觀孔隙度(%) | 18.8 | 19.9 | 20.6 | 19.9 | 20.5 | 22.4 | 18.0 | |
冷抗碎強度(MPa) | 50 | 70 | 72 | 61 | 50 | 37 | 112 | |
在1550 °C, 負載0.2 Mpa的潛變; Z 5-25(%) | - 0.19 | - 0.19 | - 0.09 | - 0.10 | - 0.21 | - 0.15 | - 0.21 |
已發現,根據本發明的燒製磚表現優良的潛變行為(Z
5-25-值,25 h及5 h之間的測試期間的變形),至少等同於傳統高燒製及高純度剛玉磚(參考)。
圖
1 a及
1 b顯示本發明實施例1的微結構,圖
2 a及
2 b顯示本發明實施例4的微結構,圖
3 a及
3 b顯示本發明實施例6的微結構。可以看到支架晶粒(100)、含有YAG (102)或Y-FSZ (103)或二者的黏結基質(101)以及開放型孔隙(104)。
為了以定量方式評量對含有蒸汽、氫氣和碳氧化物的還原熱氣體的改進的高抵抗性,將如實施例1至6所述製備的根據本發明的磚在用於工業製造合成氣的容器的燃燒室中使用催化製程進行比較實際試驗約7個月。最高應用溫度約為1200°C。將如上所述製備的傳統高純度剛玉磚(參考)用作比較材料。在試驗前後量測所有待測磚的重量,並確定相應的重量損失百分比。在此基礎上,根據以下方程式計算比較重量損失百分比(CWL):
CWL (%) = (實施例重量損失(%)∙100 %) / (參考重量損失(%))。
結果列在表2,也顯示在圖4的圖表。
表2
實施例 項目 | 1 | 2 | 3 | 4 | 5 | 6 | 參考 |
比較重量損失CWL (%) | 60.2 | 52.5 | 40.1 | 59.4 | 74.6 | 48.7 | 100 |
表2所示結果反映根據本發明的製品在對含有蒸汽、氫氣和碳氧化物的熱氣體的抵抗性方面明顯優於高純度剛玉磚。關於實施例4至6,檢測不到立方氧化鋯相與試驗相關的不穩定。
還出人意料地發現,根據本發明的製品的熱傳導率明顯低於市售的剛玉磚的熱傳導率,這尤其對節能具有正面效應。
[圖1a]至[圖3b]顯示耐火製品的具體實例的微觀結構。
[圖4]顯示與傳統的高燒製和高純度剛玉磚相比,耐火製品的具體實例在長期暴露於含有蒸汽的還原熱氣體之後的重量損失。
100:支架晶
101:黏結基質
104:開放型孔隙
Claims (13)
- 一種成型及燒製的粗陶瓷耐火製品,其包含 (a) 化學組成物,其包含以下含量:Al 2O 3:至少40 wt.%;Y 2O 3: 2.0-57 wt.%;ZrO 2:低於42.0 wt.%;及 (b) 黏結基質,其至少包含具有三元系統Al 2O 3-Y 2O 3-ZrO 2立方改性的含氧化釔的結晶混合氧化物。
- 如請求項1之耐火製品,其中具有三元系統的立方晶體結構的該含氧化釔的結晶混合氧化物係釔鋁石榴石(Y 3Al 5O 12)。
- 如請求項1之耐火製品,其中具有立方晶體結構的該含氧化釔的結晶混合氧化物係氧化釔完全穩定的氧化鋯,或氧化釔完全穩定的氧化鋯及Y 3Al 5O 12的混合物。
- 如請求項1至3中任一項之耐火製品,其中該製品中進一步含有的氧化物SiO 2、TiO 2、Fe 2O 3、鹼和HfO 2的總和最多2.2 wt.%,較佳最多1.7 wt.%。
- 如請求項1至4中任一項之耐火製品,其中該化學組成物包含至少60 wt. %的Al 2O 3。
- 如請求項1至5中任一項之耐火製品,其中該化學組成物包含2.0至25 wt. %之間的Y 2O 3。
- 一種製備成型及燒製的粗陶瓷耐火物之方法,該粗陶瓷耐火物包含化學組成物,該化學組成物包含以下含量:Al 2O 3:至少40 wt.%;Y 2O 3:2.0-57 wt.%;ZrO 2:低於42.0 wt.%,該方法包含以下步驟: 提供黏結基質,其至少包含具有三元系統Al 2O 3-Y 2O 3-ZrO 2立方改性的含氧化釔的結晶混合氧化物。
- 如請求項7之方法,其中用於提供該含氧化釔的結晶混合氧化物的Y 2O 3的純度係Y 2O 3/稀土氧化物總量,該純度>98.5%,諸如>99%或諸如99.9%。
- 如請求項7或8之方法,其中原料混合物包含顆粒狀高純度熔融剛玉及/或燒結剛玉,其具有> 98.5 wt. %、較佳 > 99 wt. %、最佳 > 99.5 wt. %的Al 2O 3含量且具有0-1 mm之間及/或1-5 mm之間的晶粒尺寸。
- 如請求項7至9中任一項之方法,其中該黏結基質係在該原料混合物成型後燒製該原料混合物而形成。
- 如請求項7至10中任一項之方法,其中該Y 2O 3的平均晶粒尺寸小於 63 µm,諸如小於25 µm或諸如小於10 µm。
- 一種如請求項1至6中任一項之製品之用途,其係作為暴露於還原氣氛的耐火材料。
- 一種用於製備富含氫氣和一氧化碳的氣體的容器,該容器包含請求項1至6中任一項之製品。
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