CN108341666A - 一种匣钵及其制备方法 - Google Patents
一种匣钵及其制备方法 Download PDFInfo
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- mullite
- alumina
- potassium aluminate
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 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 33
- 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 33
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 33
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 31
- 239000010431 corundum Substances 0.000 claims abstract description 21
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 20
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 11
- WPUINVXKIPAAHK-UHFFFAOYSA-N aluminum;potassium;oxygen(2-) Chemical compound [O-2].[O-2].[Al+3].[K+] WPUINVXKIPAAHK-UHFFFAOYSA-N 0.000 claims abstract 5
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000007767 bonding agent Substances 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 11
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 11
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 11
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 11
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 7
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 7
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 150000004676 glycans Chemical class 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 229920001282 polysaccharide Polymers 0.000 claims description 3
- 239000005017 polysaccharide Substances 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 229920000609 methyl cellulose Polymers 0.000 claims 1
- 239000001923 methylcellulose Substances 0.000 claims 1
- 239000010406 cathode material Substances 0.000 abstract description 10
- 230000035939 shock Effects 0.000 abstract description 10
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052700 potassium Inorganic materials 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- KVOIJEARBNBHHP-UHFFFAOYSA-N potassium;oxido(oxo)alumane Chemical compound [K+].[O-][Al]=O KVOIJEARBNBHHP-UHFFFAOYSA-N 0.000 description 17
- 238000000034 method Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 230000003628 erosive effect Effects 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 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 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- OVAQODDUFGFVPR-UHFFFAOYSA-N lithium cobalt(2+) dioxido(dioxo)manganese Chemical compound [Li+].[Mn](=O)(=O)([O-])[O-].[Co+2] OVAQODDUFGFVPR-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
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Abstract
本发明提供一种匣钵，包含以下重量百分比的原料：65‑87％的莫来石、5‑10％的刚玉、3‑7％的活性α‑氧化铝及5‑10％的合成铝酸钾；所述合成铝酸钾的化学组成中包含重量百分比分别为92.0‑93.0％的Al2O3与7.0‑8.0％的K2O。所述匣钵具备较强的抗热震和抗侵蚀能力，能够用于煅烧三元正极材料。本发明还提供一种匣钵的制备方法。
Description
【技术领域】
本发明属于耐火材料技术领域，尤其涉及一种匣钵及其制备方法。
【背景技术】
锂离子电池因其具备储存能量、可快速充放电、循环寿命长、环境友好等特点得到了广泛应用。正极材料是决定锂离子电池性能的关键因素之一，而镍钴锰酸锂等三元材料因具有高比容量、长循环等优势成为应用前景最好的正极材料。现有技术中，三元正极材料通常采用前驱体在900-1100℃的温度下烧制而成，煅烧过程中用来盛装前驱体的匣钵对烧成工艺至关重要。
煅烧制备三元正极材料过程中，匣钵不仅受到急冷急热的热应力冲击，还承受着三元正极材料的侵蚀，其中，锂氧化物的渗透侵蚀是匣钵损毁的主要原因。目前，大多采用莫来石、堇青石及尖晶石材料制备匣钵，并添加氧化镁等碱性成分来提高抗锂侵蚀能力。然而引入氧化镁、尖晶石等材料制备的匣钵热膨胀率增大，导致抗热震能力降低。此外，相对于锰酸锂、钴酸锂等一元正极材料，三元正极材料的侵蚀实际上为多元侵蚀，其中的碱性锂离子在煅烧温度下异常活跃，渗透性增强，并且在多元体系中存在共熔点，形成液相进而加速了侵蚀渗透。另一方面，三元正极材料与匣钵材料在高温下发生化学反应生成复合相，造成匣钵材料的热膨胀系数发生改变，局部体积发生变化，最终导致被侵蚀面发生龟裂、剥落。
鉴于此，实有必要提供一种匣钵及其制备方法以克服上述缺陷。
【发明内容】
本发明的目的在于提出一种具备较强的抗热震和抗侵蚀能力，能够用于煅烧三元正极材料的匣钵及其制备方法。
本发明提供一种匣钵，包含以下重量百分比的原料：包含以下重量百分比的原料：65-87％的莫来石、5-10％的刚玉、3-7％的活性α-氧化铝及5-10％的合成铝酸钾；所述合成铝酸钾的化学组成中包含重量百分比分别为92.0-93.0％的Al2O3与7.0-8.0％的K2O。
在一个优选实施方式中，所述莫来石的粒径为0-1.5mm；所述刚玉的粒径为0-0.044mm；所述活性α-氧化铝的粒径为0-0.005mm；所述合成铝酸钾的粒径为0-0.074mm。
在一个优选实施方式中，所述莫来石的化学组成中，Al2O3≥72.0wt％、SiO2≤27.0wt％、TiO2≤0.1wt％、Fe2O3≤0.1wt％、CaO≤0.3wt％、Na2O≤0.5wt％。
在一个优选实施方式中，所述莫来石为电熔莫来石。
在一个优选实施方式中，所述刚玉的化学组成中，Al2O3≥99.6wt％。
在一个优选实施方式中，所述活性α-氧化铝的化学组成中，Al2O3≥99.8wt％，Na2O≤0.2wt％。
在一个优选实施方式中，原料还包含结合剂；所述结合剂为羧甲基纤维素、甲基纤维素、多糖及水溶性树脂中的一种或多种。
本发明还提供一种匣钵的制备方法，包括以下步骤：
1)按照重量百分比称取莫来石、刚玉、活性α-氧化铝及合成铝酸钾，加入结合剂混合均匀，然后采用液压机成型获得匣钵坯体；
2)将液压机成型后获得的匣钵坯体送入隧道式干燥窑中进行热处理，其中，干燥窑的入口温度为40-60℃，保温区间温度为110℃，出口温度为40-60℃，热处理时间为12-24h；
3)将经过干燥热处理的匣钵坯体送入隧道窑中，在1200-1400℃的温度下保温煅烧5-8h。
本发明提供的匣钵采用莫来石、刚玉、活性α-氧化铝及合成铝酸钾制成，存在以下有益效果：其一是合成铝酸钾的热膨胀较低，可以进一步提高莫来石质匣钵的体积稳定性，从而提高匣钵的抗热震能力；其二是合成铝酸钾中含有的少量钾离子与三元正极材料中的锂离子同属碱性离子，两者不容易发生反应，能够显著降低三元正极材料对匣钵的液相渗透，从而提高匣钵的抗侵蚀能力；其三是含有合成铝酸钾的匣钵与三元正极材料接触不反应，能够防止三元正极材料在煅烧过程中被污染或与匣钵粘结，提高合格率。
【附图说明】
图1为本发明提供的匣钵的制备方法的流程框图。
【具体实施方式】
本发明提供一种匣钵，包含以下重量百分比的原料：65-87％的莫来石、5-10％的刚玉、3-7％的活性α-氧化铝及5-10％的合成铝酸钾。具体的，所述合成铝酸钾的化学组成中包含重量百分比分别为92.0-93.0％的Al2O3与7.0-8.0％的K2O。
更为具体的，所述莫来石的化学组成中，Al2O3≥72.0wt％、SiO2≤27.0wt％、TiO2≤0.1wt％、Fe2O3≤0.1wt％、CaO≤0.3wt％、Na2O≤0.5wt％；所述刚玉的化学组成中，Al2O3≥99.6wt％；所述活性α-氧化铝的化学组成中，Al2O3≥99.8wt％，Na2O≤0.2wt％。
在一个实施例中，所述莫来石的粒径为0-1.5mm；所述刚玉的粒径为0-0.044mm；所述活性α-氧化铝的粒径为0-0.005mm；所述合成铝酸钾的粒径为0-0.074mm，使原料具有合理的颗粒级配。
在一个实施例中，所述莫来石优选为电熔莫来石。需要说明的是，莫来石常规生产工艺包括电熔法和烧结法，与烧结法制备的莫来石相比，电熔莫来石晶粒大且发育更加完善，性能较为稳定。
进一步的，所述匣钵的原料还包含结合剂，所述结合剂优选为羧甲基纤维素、甲基纤维素、多糖及水溶性树脂中的一种或多种。
请参阅图1，本发明还提供一种匣钵的制备方法，包括以下步骤：
1)按照重量百分比称取莫来石、刚玉、活性α-氧化铝及合成铝酸钾，加入结合剂混合均匀，然后采用液压机成型获得匣钵坯体；
2)将液压机成型后获得的匣钵坯体送入隧道式干燥窑中进行热处理，其中，干燥窑的入口温度为40-60℃，保温区间温度为110℃，出口温度为40-60℃，热处理时间为12-24h；
3)将经过干燥热处理的匣钵坯体送入隧道窑中，在1200-1400℃的温度下保温煅烧5-8h。
实施例1
(1)按照表1称取电熔莫来石、刚玉、活性α-氧化铝及合成铝酸钾，加入适量的水及羧甲基纤维素(结合剂)，混合均匀后采用液压机成型获得匣钵坯体，其中，羧甲基纤维素的加入量占电熔莫来石、刚玉、活性α-氧化铝及合成铝酸钾总重量的3％。
表1 实施例1中制备匣钵所需原料配方
(2)将液压机成型后获得的匣钵坯体送入隧道式干燥窑中进行热处理，其中，干燥窑的入口温度为50℃，保温区间温度为110℃，出口温度为50℃，热处理时间为18h。
(3)将经过干燥热处理的匣钵坯体送入隧道窑中，在1300℃的温度下保温煅烧5h，获得匣钵。
实施例2
(1)按照表2称取电熔莫来石、刚玉、活性α-氧化铝及合成铝酸钾，加入适量的水及羧甲基纤维素(结合剂)，混合均匀后采用液压机成型获得匣钵坯体，其中，羧甲基纤维素的加入量占电熔莫来石、刚玉、活性α-氧化铝及合成铝酸钾总重量的3％。
表2 实施例2中制备匣钵所需原料配方
(2)将液压机成型后获得的匣钵坯体送入隧道式干燥窑中进行热处理，其中，干燥窑的入口温度为50℃，保温区间温度为110℃，出口温度为50℃，热处理时间为18h。
(3)将经过干燥热处理的匣钵坯体送入隧道窑中，在1300℃的温度下保温煅烧5h，获得匣钵。
实施例3
(1)按照表3称取电熔莫来石、刚玉、活性α-氧化铝及合成铝酸钾，加入适量的水及羧甲基纤维素(结合剂)，混合均匀后采用液压机成型获得匣钵坯体，其中，羧甲基纤维素的加入量占电熔莫来石、刚玉、活性α-氧化铝及合成铝酸钾总重量的3％。
表3 实施例3中制备匣钵所需原料配方
(2)将液压机成型后获得的匣钵坯体送入隧道式干燥窑中进行热处理，其中，干燥窑的入口温度为50℃，保温区间温度为110℃，出口温度为50℃，热处理时间为18h；
(3)将经过干燥热处理的匣钵坯体送入隧道窑中，在1300℃的温度下保温煅烧5h，获得匣钵。
对比例
(1)按照表4称取电熔莫来石、刚玉及活性α-氧化铝，加入适量的水及羧甲基纤维素(结合剂)，混合均匀后采用液压机成型获得匣钵坯体，其中，羧甲基纤维素的加入量占电熔莫来石、刚玉及活性α-氧化铝总重量的3％；
表4 对比例中制备匣钵所需原料配方
(2)将液压机成型后获得的匣钵坯体送入隧道式干燥窑中进行热处理，其中，干燥窑的入口温度为50℃，保温区间温度为110℃，出口温度为50℃，热处理时间为18h；
(3)将经过干燥热处理的匣钵坯体送入隧道窑中，在1300℃的温度下保温煅烧5h，获得匣钵。
对实施例1-3及对比例制备的匣钵进行体积密度测试、显气孔率测试、抗热震性能测试及抗侵蚀性能测试，结果如表5所示。抗热震性能的测试方法具体如下：将待测匣钵迅速放入炉温为1000℃的马弗炉中，使其在1000℃的温度下保温15min，取出后迅速放入5-50℃的流动水中完成一次热震，接下来将完成热震的匣钵放入110℃的烘干箱内烘干，冷却至室温后测量抗折强度并计算抗折强度保持率。此外，抗侵蚀性能测试中，采用静态坩埚法于1250℃的温度下保温3h。
表5 实施例1-3及对比例制备的匣钵的性能测试结果
实施例1-3及对比例制备的匣钵进行的抗热震性能测试和抗侵蚀性能测试结果表明：与对比例制备的匣钵相比较，由实施例1-3制备的匣钵具有更好的抗热震能力和抗侵蚀能力。
以上所述仅为本发明的较佳实施例而已，是结合具体的优选实施方式对本发明所作的进一步详细说明，不能认定本发明的具体实施局限于这些说明。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围内。
Claims (8)
1.一种匣钵，其特征在于，包含以下重量百分比的原料：65-87％的莫来石、5-10％的刚玉、3-7％的活性α-氧化铝及5-10％的合成铝酸钾；所述合成铝酸钾的化学组成中包含重量百分比分别为92.0-93.0％的Al2O3与7.0-8.0％的K2O。
2.根据权利要求1所述的匣钵，其特征在于，所述莫来石的粒径为0-1.5mm；所述刚玉的粒径为0-0.044mm；所述活性α-氧化铝的粒径为0-0.005mm；所述合成铝酸钾的粒径为0-0.074mm。
3.根据权利要求1所述的匣钵，其特征在于，所述莫来石的化学组成中，Al2O3≥72.0wt％、SiO2≤27.0wt％、TiO2≤0.1wt％、Fe2O3≤0.1wt％、CaO≤0.3wt％、Na2O≤0.5wt％。
4.根据权利要求3所述的匣钵，其特征在于，所述莫来石为电熔莫来石。
5.根据权利要求1所述的匣钵，其特征在于，所述刚玉的化学组成中，Al2O3≥99.6wt％。
6.根据权利要求1所述的匣钵，其特征在于，所述活性α-氧化铝的化学组成中，Al2O3≥99.8wt％，Na2O≤0.2wt％。
7.根据权利要求1-6任意一项所述的匣钵，其特征在于，原料还包含结合剂；所述结合剂为羧甲基纤维素、甲基纤维素、多糖及水溶性树脂中的一种或多种。
8.根据权利要求7所述的匣钵的制备方法，其特征在于，包括以下步骤：
1)按照重量百分比称取莫来石、刚玉、活性α-氧化铝及合成铝酸钾，加入结合剂混合均匀，然后采用液压机成型获得匣钵坯体；
2)将液压机成型后获得的匣钵坯体送入隧道式干燥窑中进行热处理，其中，干燥窑的入口温度为40-60℃，保温区间温度为110℃，出口温度为40-60℃，热处理时间为12-24h；
3)将经过干燥热处理的匣钵坯体送入隧道窑中，在1200-1400℃的温度下保温煅烧5-8h。
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