CN107892581A - 一种高强抗腐锆刚玉蜂窝陶瓷体及其制备方法 - Google Patents
一种高强抗腐锆刚玉蜂窝陶瓷体及其制备方法 Download PDFInfo
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- CN107892581A CN107892581A CN201711210573.7A CN201711210573A CN107892581A CN 107892581 A CN107892581 A CN 107892581A CN 201711210573 A CN201711210573 A CN 201711210573A CN 107892581 A CN107892581 A CN 107892581A
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- honeycomb ceramic
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- fused alumina
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000000919 ceramic Substances 0.000 title claims abstract description 70
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 22
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 21
- 239000004927 clay Substances 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 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 claims abstract description 18
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 17
- 238000007603 infrared drying Methods 0.000 claims abstract description 17
- 239000000314 lubricant Substances 0.000 claims abstract description 17
- 239000004014 plasticizer Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- 238000001125 extrusion Methods 0.000 claims abstract description 11
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 11
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 8
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 8
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims abstract description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 12
- 239000002383 tung oil Substances 0.000 claims description 9
- 239000007767 bonding agent Substances 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 7
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 6
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 6
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 6
- 229920000609 methyl cellulose Polymers 0.000 claims description 6
- 239000001923 methylcellulose Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 5
- 229910000831 Steel Inorganic materials 0.000 abstract description 4
- 238000010304 firing Methods 0.000 abstract description 4
- 239000010959 steel Substances 0.000 abstract description 4
- 239000003921 oil Substances 0.000 abstract description 3
- 241000264877 Hippospongia communis Species 0.000 description 50
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 9
- 239000000395 magnesium oxide Substances 0.000 description 9
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
- 239000010431 corundum Substances 0.000 description 6
- 238000005336 cracking Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910052594 sapphire Inorganic materials 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 230000007774 longterm Effects 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- 229910052845 zircon Inorganic materials 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- QRRWWGNBSQSBAM-UHFFFAOYSA-N alumane;chromium Chemical compound [AlH3].[Cr] QRRWWGNBSQSBAM-UHFFFAOYSA-N 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052878 cordierite Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012797 qualification Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910006501 ZrSiO Inorganic materials 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000005445 natural material Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052849 andalusite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- JUVGUSVNTPYZJL-UHFFFAOYSA-N chromium zirconium Chemical compound [Cr].[Zr] JUVGUSVNTPYZJL-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 235000012907 honey Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052850 kyanite Inorganic materials 0.000 description 1
- 239000010443 kyanite Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052851 sillimanite Inorganic materials 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical compound [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C04B38/0006—Honeycomb structures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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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- C04B2235/9676—Resistance against chemicals, e.g. against molten glass or molten salts against molten metals such as steel or aluminium
Abstract
本发明提供一种高强抗腐锆刚玉蜂窝陶瓷体及其制备方法，将如下重量百分比的原料组分：刚玉粉35‑40％、a‑Al2O3粉15‑20％、c‑ZrO2粉8‑10％、莫来石粉5‑10％、高岭土5‑10％、粘土粉8‑12％、Li2O粉0.5‑1.0％、MgO粉0.3‑0.5％；粘结剂3‑5％、润滑剂3‑5％、增塑剂0.2‑0.5％；采用干法球磨工艺使原料细化，然后采用湿法混炼获得泥料；泥料真空挤制成型，坯体红外干燥：坯体烧成即得；烧成过程以40℃/h缓慢程序升温至400℃，然后以100‑120℃/h的速度升温至最高烧成温度，在1600‑1750℃高温下的烧成时间为4‑8h。本发明制得的高强抗腐锆刚玉蜂窝陶瓷体能保证其具有高的使用温度(1500℃)和热容量基础上，改善其热学、力学性能和耐腐蚀性，其使用寿命可达20‑24个月；可广泛应用于钢铁、石油、化工等行业的各种蓄热式加热炉中。
Description
技术领域
本发明涉及蜂窝陶瓷技术领域，具体涉及一种高强抗腐锆刚玉陶瓷体及其制备方法。
背景技术
在钢铁、石化等行业都会用到各种蓄热式工业加热炉，作为蓄热式工业加热炉中的关键部件—陶瓷蓄热体，其蓄热式加热炉性能指标和热效率的高低直接取决于陶瓷蓄热体的性能。蜂窝陶瓷体是蓄热式工业加热炉理想的陶蓄热材料，它既能提高燃烧效果，节约能源，又能减少有害气体排放，降低环境污染。蜂窝陶瓷蓄热体具有耐高温、热稳定性好、蓄热量大、导热性能好等显著的优点，以蜂窝陶瓷作为热交换介质，最大限度地回收烟气的热量，节省燃料，降低排放烟气的温度，减少NOX气体的排放，降低工业窑炉的氧化烧损，在环保节能的蓄热式高温空气燃烧技术领域有广泛的应用。目前市场上的蜂窝陶瓷蓄热材料在使用过程中，如堇青石、莫来石和刚玉莫来石存在使用寿命有限、不耐腐蚀、耐火温度较低、陶瓷体表面层易开裂脱落等问题，不能满足工业应用中的工作需要。
对比文件1：CN103204690A公开一种锆质蜂窝陶瓷体，包括下列原料组份：10-50％的陶瓷原料、10-50％的α-Al2O3粉、10-30％的粘土、3-10％的MgO、3-8％的有机纤维素、3-7％的粘合剂和3-7％的ZrO2粉，经球磨混碾、挤出成型、干燥焙烧而成。
对比文件2：CN101125751A公开一种锆铬刚玉质新型蜂窝陶瓷蓄热体，包括刚玉质新型蜂窝陶瓷体由刚玉粉、α-Al2O3粉、粘土、MgO、有机纤维素、桐油、Cr2O3粉和ZrO2粉组成；其各组份的重量百分比为：刚玉粉40-50％，α-Al2O3粉20-30％，粘土5-10％，MgO3-10％，有机纤维素3-8％，桐油3-7％，Cr2O3粉3-7％，ZrO2粉3-7％；将上述各组份按比例配制混碾成型后煅烧而成。
对比文件3：CN101066881A公开一种用铝铬渣制成的蜂窝陶瓷原料及其制作蜂窝陶瓷的生产工艺，蜂窝陶瓷原料是在铝铬渣细粉中加入铝铬渣细粉量1-80％的莫来石或堇青石或硅线石、红柱石、蓝晶石的三石混合物和6-10％的粘接剂组成；将上述原料配料、混合球磨、加粘结剂和水捏合、进行真空练泥、挤压成型、干燥、烧成蜂窝陶瓷。
上述对比文件1-对比文件3中，存在的缺陷：上述对比文件提供的蜂窝陶瓷的生产工艺中多采用湿法球磨(在球磨过程中加水)，不能保证球磨粒度的均匀性；此外上述对比文件提供原料组分体系及生产工艺制得的蜂窝陶瓷体其热学、力学性能、耐腐蚀性及使用寿命都还有待提高。且上述对比文件提供的制备工艺的产品成形和烧成合格率也都不高。
发明内容
本发明要解决的技术问题是提供一种高强抗腐锆刚玉蜂窝陶瓷体及其制备方法，该制备方法能有效地提高产品的成形和烧成合格率，使用该制备方法制得的高强抗腐锆刚玉蜂窝陶瓷体能保证其具有高的使用温度(1500℃长期使用)和高的热容量基础上，改善其热学、力学性能和耐腐蚀性，显著延长其使用寿命；可以广泛应用于钢铁、石油、化工等行业的各种蓄热式加热炉中，比目前其他的蓄热材料如堇青石、莫来石和刚玉莫来石在使用寿命，耐火度等关键参数上都有大幅度提高。
为了解决上述技术问题，本发明采用以下技术方案：
提供一种高强抗腐锆刚玉蜂窝陶瓷体，包括如下重量百分比的原料组分：
刚玉粉35-40％、a-Al2O3粉15-20％、c-ZrO2粉8-10％、莫来石粉5-10％、高岭土5-10％、粘土粉8-12％、Li2O粉0.5-1.0％、MgO粉0.3-0.5％；粘结剂3-5％、润滑剂3-5％、增塑剂0.2-0.5％。
优选地，
所述粘接剂为：甲基纤维素、羟丙基纤维素或其结合。
优选地，
所述润滑剂为：硬脂酸、桐油或其组合。
优选地，
所述增塑剂为甘油。
本发明还提供一种上述高强抗腐锆刚玉蜂窝陶瓷体的制备方法，具体包括如下步骤：
(1)混合球磨：将如下重量百分比的原料组分：刚玉粉35-40％、a-Al2O3粉15-20％、c-ZrO2粉8-10％、莫来石粉5-10％、高岭土5-10％、粘土粉8-12％、Li2O粉0.5-1.0％、MgO粉0.3-0.5％；粘结剂3-5％、润滑剂3-5％、增塑剂0.2-0.5％；
采用干法球磨工艺使原料细化，然后采用湿法混炼获得泥料；
(2)真空挤制成型：将泥料放入真空练泥机中进行炼泥后，再放入挤压成型机中挤压成型得坯体；真空度控制在0.08-0.5MPa；
(3)红外干燥：将挤压成型的坯体进行红外干燥，得蜂窝陶瓷体干坯；
(4)坯体烧成：将蜂窝陶瓷体干坯装入煅烧炉中，煅烧炉煅烧过程中以40℃/h缓慢程序升温至400℃，然后以100-120℃/h的速度升温至最高烧成温度，在1600-1750℃高温下的烧成时间为4-8h；
(5)随炉冷却或空冷至常温出炉，即得。
进一步地，
步骤(3)中：红外干燥采用远红外干燥箱进行干燥，干燥温度为120-150℃；干燥时间为：0.5-1h。
进一步地，
步骤(1)中的干法球磨时间为10-12h。
进一步地，
步骤(1)中还包括：先对粘土进行淘洗处理。
优选地，
所述粘接剂为：甲基纤维素、羟丙基纤维素或其结合。
优选地，
所述润滑剂为：硬脂酸、桐油或其组合。
优选地，
所述增塑剂为甘油。
本发明的有益效果：
1、配方体系创新：在高温稳定、高比重的α-Al2O3和c-ZrO2主晶相基础上，加入部份莫来石晶相和粘土及少量锂质、镁质原料。在高强抗腐蚀锆刚玉蜂窝陶瓷中引入ZrO2，一方面可以增加ZrO2的比重，二是对α-Al2O3起到增韧和增强的效果，三是可以抑制刚玉晶粒过分长大，同时原位形成部份ZrSiO4晶相，在增加热膨胀系数小的晶相的同时有效减少材料中的热膨胀系数大的游离SiO2；在保证高的使用温度(1500℃长期使用)和高的热容量基础上，改善高强抗腐蚀锆刚玉蜂窝陶瓷的热学、力学性能和耐腐蚀性，显著延长其使用寿命。
2、显微结构热应力匹配设计创新：由于Al2O3的热膨胀系数(α＝8×10-6/℃)和ZrO2的热膨胀系数(α＝7.0×10-6/℃)都较大，高强抗腐蚀锆刚玉蜂窝陶瓷在坯体烧制过程中合理引入的莫来石晶相(α＝5.3×10-6/℃)和通过原位形成的ZrSiO4晶相(α＝4.5x10-6/℃)的热膨胀系数都较小，使得主晶相的热膨胀系数渐变，复合材料界面残余热应力减小，对复合材料系统的抗热震性可以起到很好的缓和作用，有效地解决“开裂”缺陷，提高高强抗腐蚀锆刚玉蜂窝陶瓷体的使用寿命。
3、优化高强抗腐蚀锆刚玉蜂窝陶瓷体的Li2O-Al2O3-SiO2、MgO-Al2O3-SiO2和K2O-Al2O3-SiO2三元体系低共熔的复合熔剂，达到混合离子效应，实现高强抗腐蚀锆刚玉蜂窝陶瓷体的较宽烧成范围致密化和高比重，改善耐腐蚀性、蓄热性和热、力学性能；
4、优化研制粘结剂、增塑剂、润滑剂等成形剂组合，有效地提高产品的成形和烧成合格率。
5、一系列制备工艺创新：
(1)为减少天然原料中混入的游离石英，采用易行有效的淘洗粘土方法：先对粘土进行淘洗处理，除掉粘土天然原料中可能混有的游离石英；
(2)采用干法球磨与湿法混练相结合的工艺技术方案，提高密度差大原料混合的均匀度，并合理控制原料粒度分布；
(3)采用真空挤制，以确保成型产品的密度和均匀性。
(4)采用红外干燥，由于红外线的穿透能力强，能实现坯体均匀快速干燥，在干燥过程中基本没有出现产品变形、开裂的现象，干燥合格率达到98％以上，与传统干燥方法比，干燥时间缩短40-50％，干燥能耗节省约25-30％。
(5)优化控制烧成制度，确定合理的保温时间，促进晶相发育完整，有效地提高高强抗腐蚀锆刚玉蜂窝陶瓷体的各项热学、力学性能和耐腐蚀性能指标，在防堵塞、抗裂和耐腐蚀等方面明显优于现有其他蜂窝陶瓷产品，使用寿命长达20-24个月。
综上，本发明制得的高强抗腐锆刚玉蜂窝陶瓷体能保证其具有高的使用温度(1500℃长期使用)和高的热容量基础上，改善其热学、力学性能和耐腐蚀性，显著延长其使用寿命；可以广泛应用于钢铁、石油、化工等行业的各种蓄热式加热炉中，比目前其他的蓄热材料如堇青石、莫来石和刚玉莫来石在使用寿命，耐火度等关键参数上都有大幅度提高。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明实施例1坯料粒径大小粒度分布图；
图2为本发明实施例1坯体烧成过程的DSC-TG曲线图；
图3为本发明实施例1锆刚玉蜂窝陶瓷坯体在1600℃保温2h的显微结构电镜图；
图4为本发明实施例1锆刚玉蜂窝陶瓷坯体在1600℃保温7h的显微结构电镜图；
图5为本发明实施例1锆刚玉蜂窝陶瓷坯体烧结前生坯的晶体结构分析-X射线粉末衍射图(XRD)；
图6为本发明实施例1锆刚玉蜂窝陶瓷坯体烧成后的晶体结构分析-X射线粉末衍射图(XRD)。
具体实施方式
下面结合实施例及附图对发明进一步说明，但不用来限制本发明的范围。
实施例1
本实施例提供一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，具体包括如下步骤：
(1)混合球磨：准备如下重量百分比的原料组分：刚玉粉35％、a-Al2O3粉15％、c-ZrO2粉10％、莫来石粉10％、高岭土10％、粘土粉12％、Li2O粉0.5％、MgO粉0.3％，粘结剂4％、润滑剂3％、增塑剂0.2％；
本实施例中：
粘接剂采用：甲基纤维素及羟丙基纤维素的结合物；
润滑剂采用：硬脂酸与桐油的结合物；
增塑剂采用甘油；
球磨前先对粘土粉进行淘洗处理，除去原料中可能含有的游离石英；
将上述质量百分比的原料组分采用干法球磨工艺球磨10h，使原料细化；
如图1的粒度分布图所示：球磨10h后坯料平均粒径D50为14.67μm，D98仅39.55μm。98％的颗粒小于40μm，最大颗粒不超过55μm，因而可以较好地保证产品的一致性和均匀性。
然后将球磨后的粉料采用湿法混炼获得泥料；
(2)真空挤制成型：将泥料放入真空练泥机中进行炼泥后，再放入挤压成型机中挤压成型得坯体；真空度控制在0.08MPa以上，以确保成型产品的密度和均匀性；
(3)红外干燥：将挤压成型的坯体进行红外干燥，得蜂窝陶瓷体干坯；
红外干燥采用远红外干燥箱进行干燥，干燥温度为120℃；干燥1h；
(4)坯体烧成：将蜂窝陶瓷体干坯装入煅烧炉中，煅烧炉煅烧过程中以40℃/h缓慢程序升温至400℃，然后以100-120℃/h的速度升温至最高烧成温度，在1600℃高温下保温7h；
(5)随炉冷却或空冷至常温出炉，即得成品高强抗腐锆刚玉蜂窝陶瓷体。
将本实施例制得的高强抗腐锆刚玉蜂窝陶瓷体进行检测，其DSC-TG曲线图(热重曲线TG，差示扫描量热曲线DSC)如图2所示，
其化学组成如下表1所示：
表1锆刚玉蜂窝陶瓷蓄热体的化学组成分析结果
如表1所示，其中Al2O3含量达到64.1％，ZrO2含量为8.5％。
在烧结过程中，观察其晶体显微结构，图3、图4分别为本实施例1锆刚玉蜂窝陶瓷坯体在1600℃保温2h及1600℃保温7h的显微结构电镜图；
本实施例还对产品烧结前后进行了X射线衍射分析，图5、图6分别为本实施例锆刚玉蜂窝陶瓷坯体烧成前的生坯的晶体结构分析-X射线粉末衍射图(XRD)、烧成后的晶体结构分析-X射线粉末衍射图(XRD)。
由图5、6对比可知，烧成前生坯的晶相由所用原料的刚玉、莫来石和氧化锆(ZrO2)组成，烧成后的产品中除原有的物相外，增加了少量硅酸锆(ZrSiO4)相，是烧成过程中氧化锆与结合粘土中分解形成游离SiO2反应的结果。
图5产品烧结前后的X射线衍射分析结果锆刚玉蜂窝陶瓷蓄热体产品的典型显微结构如图4所示(同一位置不同放大分辨率)：产品的显微结构较均匀，气孔较少且尺寸不超过10微米，最大晶粒尺寸也仅20微米左右，形成了锆刚玉颗粒状晶体与莫来石条状晶体相互交织的致密的显微结构，因而能使材料获得较好的强韧化效果。
经检测，本实施例制得的的技术性能指标如下表2所示：
表2技术性能指标情况表
本实施例在高温稳定、高比重的α-Al2O3和c-ZrO2主晶相基础上，加入部份莫来石晶相和粘土及少量锂质、镁质原料。本实施例中引入ZrO2，一方面可以增加ZrO2的比重，二是对α-Al2O3起到增韧和增强的效果，三是可以抑制刚玉晶粒过分长大，同时原位形成部份ZrSiO4晶相，在增加热膨胀系数小的晶相的同时有效减少材料中的热膨胀系数大的游离SiO2；在保证高的使用温度(1500℃长期使用)和高的热容量基础上，改善高强抗腐蚀锆刚玉蜂窝陶瓷的热学、力学性能和耐腐蚀性，显著延长其使用寿命。
由于Al2O3的热膨胀系数(α＝8×10-6/℃)和ZrO2的热膨胀系数(α＝7.0×10-6/℃)都较大，本实施例在坯体烧制过程中合理引入的莫来石晶相(α＝5.3×10-6/℃)和通过原位形成的ZrSiO4晶相(α＝4.5x10-6/℃)的热膨胀系数都较小，使得主晶相的热膨胀系数渐变，复合材料界面残余热应力减小，对复合材料系统的抗热震性可以起到很好的缓和作用，有效地解决“开裂”缺陷，提高高强抗腐蚀锆刚玉蜂窝陶瓷体的使用寿命。
本实施例中形成Li2O-Al2O3-SiO2、MgO-Al2O3-SiO2和K2O-Al2O3-SiO2三元体系低共熔的复合熔剂，能达到混合离子效应，实现高强抗腐蚀锆刚玉蜂窝陶瓷体的较宽烧成范围致密化和高比重，改善耐腐蚀性、蓄热性和热、力学性能。
通过研制粘结剂、增塑剂、润滑剂等成形剂组合，有效地提高产品的成形和烧成合格率。
此外工艺中采用红外干燥，由于红外线的穿透能力强，能实现坯体均匀快速干燥，在干燥过程中基本没有出现产品变形、开裂的现象，干燥合格率达到98％以上，与传统干燥方法比，干燥时间缩短40-50％，干燥能耗节省约25-30％。
通过控制烧成制度，确定合理的保温时间，促进晶相发育完整，有效地提高高强抗腐蚀锆刚玉蜂窝陶瓷体的各项热学、力学性能和耐腐蚀性能指标，在防堵塞、抗裂和耐腐蚀等方面明显优于现有其他蜂窝陶瓷产品，可以使其使用寿命长达20-24个月。
实施例2
本实施例提供另一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，本实施例与实施例1的区别在于：
(1)混合球磨原料组分质量百分比如下：刚玉粉40％、a-Al2O3粉20％、c-ZrO2粉8％、莫来石粉5％、高岭土5％、粘土粉10％、Li2O粉1％、MgO粉0.5％，粘结剂5％、润滑剂5％、增塑剂0.5％；
本实施例中：
粘接剂采用：甲基纤维素；润滑剂采用：桐油；增塑剂采用甘油；
(2)真空挤制成型：真空度控制在0.5MPa以上，以确保成型产品的密度和均匀性；
(3)红外干燥温度为150℃；干燥0.5h。
实施例3
本实施例提供另一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，本实施例与实施例1的区别在于：
(1)混合球磨原料组分质量百分比如下：刚玉粉38％、a-Al2O3粉18％、c-ZrO2粉9.5％、莫来石粉10％、高岭土8％、粘土粉8％、Li2O粉0.8％、MgO粉0.5％，粘结剂3％、润滑剂4％、增塑剂0.2％；
本实施例中：
粘接剂采用：羟丙基纤维素；润滑剂采用：桐油；增塑剂采用甘油；
(2)真空挤制成型：真空度控制在0.25MPa以上，以确保成型产品的密度和均匀性；
(3)红外干燥温度为140℃；干燥0.8h。
实施例2和实施例3提供的制备方法制得的锆刚玉蜂窝陶瓷体其性能参数与实施例的性能参数近似。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等同物界定。
Claims (10)
1.一种高强抗腐锆刚玉蜂窝陶瓷体，其特征在于，
包括如下重量百分比的原料组分：
刚玉粉35-40％、a-Al2O3粉15-20％、c-ZrO2粉8-10％、莫来石粉5-10％、高岭土5-10％、粘土粉8-12％、Li2O粉0.5-1.0％、MgO粉0.3-0.5％；粘结剂3-5％、润滑剂3-5％、增塑剂0.2-0.5％。
2.根据权利要求1所述的一种高强抗腐锆刚玉蜂窝陶瓷体，其特征在于，
所述粘接剂为：甲基纤维素、羟丙基纤维素或其结合。
3.根据权利要求1或2所述的一种高强抗腐锆刚玉蜂窝陶瓷体，其特征在于，
所述润滑剂为：硬脂酸、桐油或其组合。
4.根据权利要求1或2所述的一种高强抗腐锆刚玉蜂窝陶瓷体，其特征在于，
所述增塑剂为甘油。
5.一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，其特征在于，
具体包括如下步骤：
(1)混合球磨：将如下重量百分比的原料组分：刚玉粉35-40％、a-Al2O3粉15-20％、c-ZrO2粉8-10％、莫来石粉5-10％、高岭土5-10％、粘土粉8-12％、Li2O粉0.5-1.0％、MgO粉0.3-0.5％；粘结剂3-5％、润滑剂3-5％、增塑剂0.2-0.5％；
采用干法球磨工艺使原料细化，然后采用湿法混炼获得泥料；
(2)真空挤制成型：将泥料放入真空练泥机中进行炼泥后，再放入挤压成型机中挤压成型得坯体；真空度控制在0.08-0.5MPa；
(3)红外干燥：将挤压成型的坯体进行红外干燥，得蜂窝陶瓷体干坯；
(4)坯体烧成：将蜂窝陶瓷体干坯装入煅烧炉中，煅烧炉煅烧过程中以40℃/h缓慢程序升温至400℃，然后以100-120℃/h的速度升温至最高烧成温度，在1600-1750℃高温下的烧成时间为4-8h；
(5)随炉冷却或空冷至常温出炉，即得。
6.根据权利要求5所述的一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，其特征在于，
步骤(3)中：红外干燥采用远红外干燥箱进行干燥，干燥温度为120-150℃；干燥时间为：0.5-1h。
7.根据权利要求5或6所述的一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，其特征在于，
步骤(1)中的干法球磨时间为10-12h。
8.根据权利要求5或6所所述的一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，其特征在于，
步骤(1)中还包括：先对粘土进行淘洗处理。
9.根据权利要求5或6所所述的一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，其特征在于，
所述粘接剂为：甲基纤维素、羟丙基纤维素或其结合。
10.根据权利要求5或6所所述的一种高强抗腐锆刚玉蜂窝陶瓷体的制备方法，其特征在于，
所述润滑剂为：硬脂酸、桐油或其组合；
所述增塑剂为甘油。
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| CN115894015A (zh) * | 2022-11-29 | 2023-04-04 | 武汉理工大学 | 一种高强多孔陶瓷燃烧介质及其制造方法 |
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