CN112759377B - 一种锂电池正极材料焙烧用匣钵及其制备方法 - Google Patents
一种锂电池正极材料焙烧用匣钵及其制备方法 Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 34
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 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 25
- 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 21
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 21
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 15
- 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 15
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 14
- 239000011029 spinel Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 9
- 239000002689 soil Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000010304 firing Methods 0.000 claims description 12
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052642 spodumene Inorganic materials 0.000 claims description 8
- 229920001353 Dextrin Polymers 0.000 claims description 7
- 239000004375 Dextrin Substances 0.000 claims description 7
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 7
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 7
- 235000019425 dextrin Nutrition 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007790 solid phase Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 239000010406 cathode material Substances 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 230000035939 shock Effects 0.000 abstract description 12
- 230000007797 corrosion Effects 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 abstract description 11
- 239000010405 anode material Substances 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 8
- 239000003513 alkali Substances 0.000 abstract description 7
- 229910001597 celsian Inorganic materials 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000002893 slag Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- -1 Magnesium aluminate Chemical class 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000010433 feldspar Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004480 active ingredient Substances 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052850 kyanite Inorganic materials 0.000 description 1
- 239000010443 kyanite Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
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- F27—FURNACES; KILNS; OVENS; RETORTS
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- F27D5/00—Supports, screens, or the like for the charge within the furnace
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Abstract
一种锂电池正极材料焙烧用匣钵及其制备方法，属于锂电池正极材料焙烧用匣钵技术领域。目前锂电池正极材料焙烧用匣钵，主要是莫来石堇青石质材料。配方以莫来石、堇青石、氧化铝为主要原料。基质主晶相为莫来石。该类匣钵循环使用过程中因温度的变化发生开裂的现象。多数产品的循环使用10次左右就会因碱侵蚀而起皮掉渣。本发明在配方中引入碳酸钡、镁铝尖晶石、α‑氧化铝及苏州土粉料，原位合成钡长石，其基质的主晶相是钡长石，降低了基质的热膨胀系数，提高了抗热震性能；更为突出是极大的提高了匣钵的抗碱侵蚀性能。同时，由于镁铝尖晶石与莫来石堇青石热膨胀系数存在较大差别，增强了材料的韧性，提高了匣钵的抗冲击强度和抗热震性能。
Description
技术领域
一种锂电池正极材料焙烧用匣钵及其制备方法，属于锂电池正极材料焙烧用匣钵技术领域。
背景技术
匣钵是在焙烧时防止产品表面被环境影响的一种硬质容器。
新能源行业的迅速发展，推动了各种新型锂电池正极材料的研究和发展，焙烧锂电池材料用的匣钵的需求量日益加大；同时对匣钵材料的性能提出了更高的要求。目前锂电池正极材料焙烧用匣钵，主要是莫来石堇青石质材料。配方以莫来石、堇青石、氧化铝为主要原料。基质主晶相为莫来石。配方中引入堇青石是为了提高材料的抗热震稳定性。该类匣钵循环使用过程中因温度的变化发生开裂的现象。多数产品的循环使用10次左右就会因碱侵蚀而起皮掉渣，该现象随使用次数的增加越来越严重，最多使用20余次就报废，因此，目前急需一种适用于锂电池正极材料焙烧的长寿命匣钵。
发明内容
本发明所要解决的技术问题是：克服现有技术的不足，提供一种抗侵蚀、抗冲击、抗热震的锂电池正极材料焙烧用匣钵及其制备方法。
本发明解决其技术问题所采用的技术方案是：一种锂电池正极材料焙烧用匣钵，其特征在于：配方中各成分按重量份组成为：碳酸钡10~15份、α-氧化铝10~20份、苏州土15~25份、莫来石15~25份、堇青石15~25份、镁铝尖晶石8~12份、锂辉石1~10份和硼酸1~3份。
本发明在配方中引入碳酸钡、α-氧化铝及苏州土粉料，通过高温烧结，原位合成钡长石，其基质的主晶相是钡长石，降低了基质的热膨胀系数，提高了抗热震性能；更为突出是极大的提高了匣钵的抗碱侵蚀性能。
在配方中引入镁铝尖晶石，可进一步强化匣钵的抗碱侵蚀性能。同时，由于镁铝尖晶石与莫来石堇青石热膨胀系数存在较大差别，增强了材料的韧性，提高了匣钵的抗冲击强度和抗热震性能。
上述比例下获得的锂电池正极材料焙烧用匣钵具有更高的抗碱侵蚀性能、韧性、抗冲击强度、抗热震性能和热震稳定性。
优选的，匣钵的化学成分按重量包括：28~33份SiO2、46~55份Al2O3、8~14份BeO及4~8份MgO，余量为杂质。过低的有效成分含量意味着没有良好的生成钡长石晶相，或者膨胀系数相差不足，优选的成分含量使最终匣钵具备更好的性能。
优选的，所述的莫来石为M70莫来石。
优选的，所述的碳酸钡、α-氧化铝和苏州土为基本材料，锂辉石、硼酸做为矿化剂。
一种上述的锂电池正极材料焙烧用匣钵制备方法，其特征在于：将原料加入结合剂后混料，用液压机液压成型后烧制完成。混料优选采用高效倾斜式混料机混料，液压成型优选的采用400T以上的双向加压液压机成型。
优选的，所述的混料中，固相与液相的质量比为3~4：1。优选的固液比能使固相在液压阶段更容易结合成型，同时在烧制阶段具备更好的挥发效果，避免吸收过多热量或使匣钵开裂。
优选的，所述的结合剂为糊精与木质素磺酸钙的水溶液。
优选的，所述的糊精与木质素磺酸钙的水溶液中糊精与木质素磺酸钙比例为1：2~4。
所述的烧制温度为500~1000℃烧制12小时，或1000~1400℃烧制8小时，或1400℃烧制6小时。充分考虑烧制过程中各原料组成的物理化学变化，并确保生成的钡长石相转化完全，结晶完善。
与现有技术相比，本发明所具有的有益效果是：以碳酸钡、α-氧化铝和苏州土做为基本原料，锂辉石、硼酸做为矿化剂，通过高温固相反应，在基质中原位合成钡长石晶相，利用钡长石高抗碱侵蚀性能和低膨胀系数的特性，提高匣钵的抗碱侵蚀性能和热震稳定性。配方中引入镁铝尖晶石、莫来石、堇青石。通过高温烧结使其与基质形成结合牢固致密的复相结构。利用镁铝尖晶石碱性较强的特性进一步提高匣钵的抗碱侵蚀性能。利用镁铝尖晶石与莫来石、堇青石热膨胀系数差别较大的特性，增强匣钵的韧性，提高匣钵的抗冲击强度和抗热震性能。
具体实施方式
下面结合实施例对本发明做进一步说明，实施例3是本发明的最佳实施例。
其中，锂辉石规格为180目，α-氧化铝规格为1000目，苏州土规格为180目，碳酸钡规格为180目。
实施例1
一种锂电池正极材料焙烧用匣钵，配方组成包括：碳酸钡6kg、α-氧化铝6.5 kg、苏州土6.5 kg、莫来石12.5 kg、堇青石11 kg、镁铝尖晶石4 kg、锂辉石2.5 kg和硼酸1 kg。
一种上述的锂电池正极材料焙烧用匣钵制备方法，将上述原料加入糊精与木质素磺酸钙按1：3组成的水溶液结合剂后，按固相与液相3：1在倾斜式混料机中混料15分钟，用400T双向加压液压机液压成型后烧制完成。烧制温度采用1200℃烧制8小时。
实施例2
一种锂电池正极材料焙烧用匣钵，配方组成包括：碳酸钡7.5kg、α-氧化铝6.5 kg、苏州土12.5kg、莫来石12.5kg、堇青石10 kg、镁铝尖晶石5 kg、锂辉石2.5kg和硼酸1 kg。
一种上述的锂电池正极材料焙烧用匣钵制备方法，在实施例1的制备方法的基础上，采用800℃烧制12小时。
实施例3
一种锂电池正极材料焙烧用匣钵，配方组成在实施例1的基础上，苏州土采用8kg。制备方法同实施例1。
实施例4
一种锂电池正极材料焙烧用匣钵，配方组成在实施例1的基础上，锂辉石采用1kg，制备方法同实施例1。
实施例5
一种锂电池正极材料焙烧用匣钵，配方组成同实施例1，制备方法中采用1200℃烧制6小时。
实施例6
一种锂电池正极材料焙烧用匣钵，配方组成同实施例1，制备方法中采用1100℃烧制12小时。
对比例1
一种锂电池正极材料焙烧用匣钵，配方组成包括：莫来石23kg，堇青石12.5kg，α-氧化铝粉3kg，苏州土4kg，蓝晶石6.5kg。
制备方法同实施例1，区别在于，采用800℃烧制12小时。
对比例2
一种锂电池正极材料焙烧用匣钵，配方组成在实施例1的基础上，不添加碳酸钡，制备方法同实施例1。
对比例3
一种锂电池正极材料焙烧用匣钵，配方组成在实施例1的基础上，不添加α-氧化铝，制备方法同实施例1。
对比例4
一种锂电池正极材料焙烧用匣钵，配方组成在实施例1的基础上，不添加镁铝尖晶石，制备方法同实施例1。
对比例5
一种锂电池正极材料焙烧用匣钵，配方组成在实施例1的基础上，不添加莫来石，制备方法同实施例1。
性能测试
取样测试最终匣钵中有效成分的含量，检测结果见下表1，表中各成分所示为所占质量百分比。其中，各成分的检验方法按耐火材料国家标准GB/T 6900-2016执行。
表1 有效成分
取样测试实施例1~6及对比例1~5体积密度、显气孔率、热震稳定性及抗侵蚀性。检测结果见下表2。
其中热震稳定性检测方法为：采用升至1100℃再水冷，至出现开裂经过的次数。
抗侵蚀性检测方法为：采用样品匣钵在1200℃焙烧钴酸锂材料，使用至底部出现侵蚀或起皮的重复次数，次数越多则抗侵蚀性越强。
表2 性能测试
根据表2实施例1~4及对比例2~5可以看出，碳酸钡、α-氧化铝、苏州土及镁铝尖晶石四种成分相辅相成，既要满足形成钡长石晶型，又要同时满足镁铝尖晶石含量能与莫来石、堇青石足以产生膨胀系数差才能使最终匣钵在各方面性能均获得显著提升。
以上所述，仅是本发明的较佳实施例而已，并非是对本发明作其它形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。
Claims (5)
1.一种锂电池正极材料焙烧用匣钵，其特征在于：配方中各成分按重量份组成为：碳酸钡10~15份、α-氧化铝10~20份、苏州土15~25份、莫来石15~25份、堇青石15~25份、镁铝尖晶石8~12份、锂辉石1~10份和硼酸1~3份；
制备方法为以下步骤：
将原料加入结合剂后混料，用液压机液压成型后烧制完成；
所述的混料中，固相与液相的质量比为3~4：1；
所述的烧制温度为1000~1400℃烧制8小时，或1400℃烧制6小时。
2.根据权利要求1所述的锂电池正极材料焙烧用匣钵，其特征在于：匣钵中化学成分按重量包括：28~33份SiO2、46~55份Al2O3、8~14份BaO及4~8份MgO，余量为杂质。
3.根据权利要求1所述的锂电池正极材料焙烧用匣钵，其特征在于：所述的莫来石为M70莫来石。
4.根据权利要求1所述的锂电池正极材料焙烧用匣钵，其特征在于：所述的结合剂为糊精与木质素磺酸钙的水溶液。
5.根据权利要求4所述的锂电池正极材料焙烧用匣钵，其特征在于：所述的糊精与木质素磺酸钙的水溶液中糊精与木质素磺酸钙比例为1：2~4。
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