CN116655394A - 一种锂电池正极材料用双层结构匣钵及其制备方法 - Google Patents
一种锂电池正极材料用双层结构匣钵及其制备方法 Download PDFInfo
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- CN116655394A CN116655394A CN202310557074.4A CN202310557074A CN116655394A CN 116655394 A CN116655394 A CN 116655394A CN 202310557074 A CN202310557074 A CN 202310557074A CN 116655394 A CN116655394 A CN 116655394A
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- sagger
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- lithium battery
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 44
- 239000010405 anode material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 33
- 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 33
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 32
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 32
- 239000005385 borate glass Substances 0.000 claims abstract description 32
- 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 32
- 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 32
- 239000002245 particle Substances 0.000 claims abstract description 32
- 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 28
- 238000009826 distribution Methods 0.000 claims abstract description 15
- 239000011029 spinel Substances 0.000 claims abstract description 13
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 23
- 238000000465 moulding Methods 0.000 claims description 16
- 239000007774 positive electrode material Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 230000006835 compression Effects 0.000 claims description 8
- 238000007906 compression Methods 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000006255 coating slurry Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000004537 pulping Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 9
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 9
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 239000010419 fine particle Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 206010067482 No adverse event Diseases 0.000 description 1
- PSMHQAOEOARJDH-UHFFFAOYSA-L [Co]=O.C([O-])([O-])=O.[Li+].[Li+] Chemical compound [Co]=O.C([O-])([O-])=O.[Li+].[Li+] PSMHQAOEOARJDH-UHFFFAOYSA-L 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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
本申请涉及锂离子电池技术领域，尤其涉及一种锂电池正极材料用双层结构匣钵及其制备方法。双层结构匣钵包括外层和内层，外层的厚度为10～15mm，内层的厚度为2‑3mm，外层采用颗粒粒径较大的原料，外层采用颗粒粒径细小的原料：外层原料为堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃；内层原料为纳米氧化锆、堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃，通过对原料颗粒粒径分布的精准控制和成型工艺中对成型模具内部进行抽真空并加压，大幅度降低了匣钵气孔率，提升其强度，进而大幅度提升匣钵使用寿命。
Description
技术领域
本申请涉及锂离子电池技术领域，尤其涉及一种锂电池正极材料用双层结构匣钵及其制备方法。
背景技术
目前堇青石-莫来石陶瓷作为窑具已得到广泛地应用，如烧结卫生洁具用的中空棚板及立柱，如煅烧各种化工原料、精细陶瓷材料、磁性材料、半导体材料用的匣钵和坩埚；特别是在作为新能源快速发展的锂电池行业，其正极材料锂盐都需要进行煅烧，所使用的堇青石-莫来石匣钵的需求量非常大，然而目前所使用的匣钵还存在诸多问题，这些问题主要表现为(1)烧成温度高，传统匣钵烧成温度达到1400摄氏度以上，甚至高达1500摄氏度，不管从能源消耗还是企业发展来说，都成为比较大的不利因素，同时也不利于国家可持续发展；(2)耐侵蚀性较差，容易与煅烧材料发生化学反应；(3)匣钵的气孔率大和抗压强度低。(4)匣钵用的原料颗粒大小分布要严格控制，导致原料的大颗粒再次粉脆会产生很多的超细粉，而超细粉又不能再次使用，导致资源的浪费。
发明内容
本申请目的在于提供一种锂电池正极材料用双层结构匣钵及其制备方法，外层采用颗粒粒径大的物料，内层采用颗粒粒径小的物料，解决物料浪费的问题，同时通过精准控制原料颗粒粒径分布，解决了上述背景技术中提出的问题。
为实现上述目的，本申请提供如下技术方案：
一种锂电池正极材料用双层结构匣钵，包括外层和内层，所述外层原材料按照质量份计，包括如下组分：堇青石10-30份，莫来石10-20份，美铝尖晶石10-40份，氧化铝10-40份，高岭土20-30份，硼酸盐玻璃10-50份；所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8目以上为20-30％，8-10目为10-20％，10-20目为10-20％，20-40目为10-20％，40-60目为5-10％，60-80目为5-10％，80-100目为5-10％；所述内层原材料按照质量份计，包括如下组分：纳米氧化锆5-10份、堇青石15-20份，莫来石15-20份，美铝尖晶石10-20份，氧化铝20-30份，高岭土20-30份，硼酸盐玻璃10-50份，所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8-10目为10-20％，10-20目为10-20％，20-40目为10-20％，40-60目为10-15％，60-80目为10-15％，80-100目为10-15％，100-325目为20-35％，所述纳米氧化锆的颗粒粒径为80-120nm。
优选的，所述外层的厚度为10～15mm，内层的厚度为2-3mm。
通过采用上述技术方案，通过对颗粒粒径分布的精准控制，原料增加粉料比例提升匣钵表面致密度及细腻度，提升匣钵使用寿命，数据化严格控制生料颗粒级配，提升堆积密度，提升匣钵强度，提升配方中碱性氧化物含量，碱性氧化物含量占20％以上，增强匣钵耐腐蚀性，提升使用寿命。匣钵外层选用颗粒粒径大的物料，保证匣钵的强度，外层选用颗粒粒径小的物料，这种搭配，保证匣钵的强度和使用寿命，同时也解决物料浪费的问题，纳米氧化锆的加入提升了匣钵耐腐蚀性能，这种双层结构也能减少纳米氧化锆用量。
优选的，所述锂电池正极材料用双层结构匣钵的气孔率为15-30％。
优选的，所述锂电池正极材料用双层结构匣钵的抗压强170-220MPa。
优选的，所述锂电池正极材料用双层结构匣钵的堆积密度2.5-4.5g/cm3。
一种锂电池正极材料用双层结构匣钵的制备方法，包括如下步骤：
S1外层混料：将堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照外层物料配方比例进行筛选、称量并混合均匀；
S2外层成型：将混合好的原料放入陶瓷匣钵的预模具中进行成型，制成匣钵生坯；
S3内层混合制浆：将内层的纳米氧化锆、堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照内层物料配方比例称量并加入20-40份水混合均匀，制成浆料；
S4内层制备，将浆料采用喷涂机涂布在所述匣钵生坯的内表面，再放入成品模具中进行成型，成型后，盖上密封盖，对成型模具内部进行抽真空并加压成型，然后进行干燥处理。
S5烧成：经过干燥后的匣钵放入烧成炉中进行烧成处理，获得锂电池正极材料用双层结构匣钵。
优选的，在步骤S4成型中，所述抽真空的真空度为800-1000Pa。
优选的，在步骤S4成型中，所述加压成型压力为400-600kgf/cm2并保压12h-14h。
优选的，在步骤S5烧结中，所述烧结温度为1200-1300℃，烧成时间为2-4小时。
通过采用上述技术方案，不仅降低了匣钵烧成温度，而且增加其热稳定性，使用寿命大大提高，可以达到40次以上。通过对成型模具内部进行抽真空并加压成型，大幅度降低了匣钵气孔率和提升其强度。
综上所述，本申请的有益技术效果：
1)烧成温度低：采用双层结构，尤其精准控颗粒粒径分布，烧成温度相比传统堇青石材料降低了200℃左右，能够减少能耗、生产成本和减少原料的浪费。
2)匣钵的使用寿命长：内层原料加入了纳米氧化锆，增加其热稳定性，使用寿命大大提高，可以达到40次以上。
3)匣钵的气孔率低和强度高：在其成型工艺中，通过对成型模具内部进行抽真空并加压成型，大幅度降低了匣钵气孔率和提升其强度。
具体实施方式
下面将结合实施例、制备例对本申请的实施方案进行详细描述，但是本领域技术人员将会理解，下列实施例仅用于说明本申请，而不应视为限制本申请的范围。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1
一种锂电池正极材料用双层结构匣钵，外层的厚度为10mm和内层的厚度为3mm，所述外层原材料按照质量份计，包括如下组分：堇青石10kg，莫来石10kg，美铝尖晶石10kg，氧化铝10kg，高岭土20kg，硼酸盐玻璃10kg；所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8目以上为20％，8-10目为20％，10-20目为10％，20-40目为20％，40-60目为10％，60-80目为10％，80-100目为10％。
内层原材料按照质量份计，包括如下组分：纳米氧化锆5kg、堇青石15kg，莫来石15kg，美铝尖晶石10kg，氧化铝20kg，高岭土20kg，硼酸盐玻璃10kg，所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8-10目为10％，10-20目为10％，20-40目为20％，40-60目为15％，60-80目为15％，80-100目为10-10％，100-325目为20％，所述纳米氧化锆的颗粒粒径为80-120nm。
实施例2
一种锂电池正极材料用双层结构匣钵，外层的厚度为15mm和内层的厚度为2mm，所述外层原材料按照质量份计，包括如下组分：堇青石30kg，莫来石20kg，美铝尖晶石40kg，氧化铝40kg，高岭土30kg，硼酸盐玻璃50kg；所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8目以上为30％，8-10目为20％，10-20目为20％，20-40目为10％，40-60目为10％，60-80目为5％，80-100目为5％。
内层原材料按照质量份计，包括如下组分：纳米氧化锆10kg、堇青石20kg，莫来石20kg，美铝尖晶石20kg，氧化铝30kg，高岭土30kg，硼酸盐玻璃50kg，所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8-10目为20％，10-20目为20％，20-40目为10％，40-60目为10％，60-80目为10％，80-100目为10％，100-325目为20％，所述纳米氧化锆的颗粒粒径为80-120nm。
实施例3
一种锂电池正极材料用双层结构匣钵，外层的厚度为13mm和内层的厚度为2.5mm，所述外层原材料按照质量份计，包括如下组分：堇青石20kg，莫来石15kg，美铝尖晶石20kg，氧化铝20kg，高岭土25kg，硼酸盐玻璃30kg；所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8目以上为25％，8-10目为15％，10-20目为15％，20-40目为15％，40-60目为10％，60-80目为10％，80-100目为10％。
内层原材料按照质量份计，包括如下组分：纳米氧化锆8kg、堇青石18kg，莫来石18kg，美铝尖晶石15kg，氧化铝25kg，高岭土25kg，硼酸盐玻璃30kg，所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8-10目为10％，10-20目为10％，20-40目为10％，40-60目为15％，60-80目为10％，80-100目为10％，100-325目为35％，所述纳米氧化锆的颗粒粒径为80-120nm。
对比例1
与实施例3相同，不同之处在于：内层原材料中，没有纳米氧化锆。
制备例1
一种锂电池正极材料用双层结构匣钵的制备方法，采用实施例1的物料，包括如下步骤：
S1外层混料：将堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照外层物料配方比例进行筛选、称量并混合均匀。
S2外层成型：将混合好的原料放入陶瓷匣钵的预模具中进行成型，制成匣钵生坯。
S3内层混合制浆：将内层的纳米氧化锆、堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照内层物料配方比例称量并加入20kg水混合均匀，制成浆料。
S4内层制备，将浆料采用喷涂机涂布在所述匣钵生坯的内表面，再放入成品模具中进行成型，成型后，盖上密封盖，对成型模具内部进行抽真空并加压成型，抽真空的真空度为800Pa，加压成型压力为400kgf/cm2并保压14h，然后进行干燥处理。
S5烧成：经过干燥后的匣钵放入烧成炉中进行烧成处理，烧成温度为1200℃，烧成时间为4小时，获得锂电池正极材料用双层结构匣钵。
制备例2
一种锂电池正极材料用双层结构匣钵的制备方法，采用实施例2的物料，包括如下步骤：
S1外层混料：将堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照外层物料配方比例进行筛选、称量并混合均匀。
S2外层成型：将混合好的原料放入陶瓷匣钵的预模具中进行成型，制成匣钵生坯。
S3内层混合制浆：将内层的纳米氧化锆、堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照内层物料配方比例称量并加入40kg水混合均匀，制成浆料。
S4内层制备，将浆料采用喷涂机涂布在所述匣钵生坯的内表面，再放入成品模具中进行成型，成型后，盖上密封盖，对成型模具内部进行抽真空并加压成型，抽真空的真空度为1000Pa，加压成型压力为600kgf/cm2并保压12h，然后进行干燥处理。
S5烧成：经过干燥后的匣钵放入烧成炉中进行烧成处理，烧成温度为1300℃，烧成时间为2小时，获得锂电池正极材料用双层结构匣钵。
制备例3
一种锂电池正极材料用双层结构匣钵的制备方法，采用实施例3的物料，包括如下步骤：
S1外层混料：将堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照外层物料配方比例进行筛选、称量并混合均匀。
S2外层成型：将混合好的原料放入陶瓷匣钵的预模具中进行成型，制成匣钵生坯。
S3内层混合制浆：将内层的纳米氧化锆、堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照内层物料配方比例称量并加入30kg份水混合均匀，制成浆料。
S4内层制备，将浆料采用喷涂机涂布在所述匣钵生坯的内表面，再放入成品模具中进行成型，成型后，盖上密封盖，对成型模具内部进行抽真空并加压成型，抽真空的真空度为900Pa，加压成型压力为500kgf/cm2并保压13h，然后进行干燥处理。
S5烧成：经过干燥后的匣钵放入烧成炉中进行烧成处理，烧成温度为1250℃，烧成时间为3小时，获得锂电池正极材料用双层结构匣钵。
制备例4
与制备例3相同，不同之处在于，采用对比例1中的物料。
制备例5
与制备例3相同，不同之处在于，在步骤S4成型中没有采用对成型模具内部进行抽真空并加压成型工艺。
性能测试
分别对制备例1-5中锂电池正极材料用双层结构匣钵进行取样，且进行其测试，数据如表1所示。
匣钵的堆积密度通过重量和体积的测算可获得。
通过液相置换法(株式会社セイシン企業，AUTO TRUE DENSER MAT-7000)测定匣钵的气孔率。
耐用次数测试：将碳酸锂粉末和氧化钴粉末按照Li和Co的摩尔比1:1在球磨机中进行1h的高速混合。将混合均匀的碳酸锂氧化钴混合物堆积至匣钵的顶部平行(大约5kg)。然后将装满混合物的匣钵放置在大电炉当中，用3h从室温升至800℃，并在800℃保持5h，然后让匣钵及其当中的锂离子电池正极材料在大电炉中自然冷却至150℃(约6h)取出，并进行观察。如果所烧的锂离子电池正极材料可以轻松从匣钵中倒出，匣钵表面没有锂离子电池正极材料残留物，并且匣钵本身没有出现开裂脱皮等不良反应，则视为匣钵可以继续进行锂离子电池正极材料的烧结实验。如果发现锂离子电池正极材料不能顺利从匣钵中倒出，或者匣钵中少量残留锂离子电池正极材料，或者匣钵本身出现开裂脱皮等状况，则视为匣钵已经到了使用寿命，终止锂离子电池正极材料的烧结实验。
强度：按照GB/T 8488-2008《陶瓷制品抗压强度试验方法》标准测定。
表1
| 堆积密度/g/cm3 | 气孔率/％ | 强度/MPa | 耐用次数/次 | |
| 制备例1 | 2.5 | 29.7 | 170.3 | 41 |
| 制备例2 | 3.3 | 24.8 | 220.8 | 48 |
| 制备例3 | 4.5 | 15.5 | 206.7 | 53 |
| 制备例4 | 4.4 | 20.2 | 212.3 | 33 |
| 制备例5 | 1.9 | 68.3 | 35.6 | 12 |
从制备例1-3分析来看，制备获得的锂电池正极材料用双层结构匣钵的堆积密度为2.5-4.5g/cm3，锂电池正极材料用双层结构匣钵的气孔率为15-30％，锂电池正极材料用双层结构匣钵的抗压强度170-220MPa，锂电池正极材料用双层结构匣钵耐用次数在40-53次。
从制备例4分析来看，内层原材料中，没有纳米氧化锆，锂电池正极材料用双层结构匣钵耐用次数从53次降为33次，纳米氧化锆对双层结构匣钵使用寿命有较大的影响。
从制备例5分析来看，在步骤S4成型中没有采用对成型模具内部进行抽真空并加压成型工艺。获得的锂电池正极材料用双层结构匣钵的堆积密度为从4.5g/cm3降为1.9g/cm3，锂电池正极材料用双层结构匣钵的气孔率为从15.5％提升到68.3％。抽真空并加压成型工艺对锂电池正极材料用双层结构匣钵的堆积密度、气孔率等指标影响非常大。
以上实施例、制备例仅用以解释说明本发明的技术方案而非对其限制，尽管上述实施例对本发明进行了具体的说明，相关技术人员应当理解，依然可对本发明的具体实施方式进行修改或者等同替换，而未脱离本发明精神和范围的任何修改和等同替换，其均应涵盖在本发明的权利要求范围之中。
Claims (9)
1.一种锂电池正极材料用双层结构匣钵，其特征在于，包括外层和内层，所述外层原材料按照质量份计，包括如下组分：堇青石10-30份，莫来石10-20份，美铝尖晶石10-40份，氧化铝10-40份，高岭土20-30份，硼酸盐玻璃10-50份；所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝 、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8目以上为20-30%，8-10目为10-20%，10-20目为10-20%，20-40目为10-20%，40-60目为5-10%，60-80目为5-10%，80-100目为5-10%；所述内层原材料按照质量份计，包括如下组分：纳米氧化锆5-10份、堇青石15-20份，莫来石15-20份，美铝尖晶石10-20份，氧化铝20-30份，高岭土20-30份，硼酸盐玻璃10-50份，所述堇青石、所述莫来石、所述美铝尖晶石、所述氧化铝 、所述高岭土和所述硼酸盐玻璃的颗粒粒径分布为：8-10目为10-20%，10-20目为10-20%，20-40目为10-20%，40-60目为10-15%，60-80目为10-15%，80-100目为10-15%，100-325目为20-35%，所述纳米氧化锆的颗粒粒径为80-120nm。
2.根据权利要求1所述一种锂电池正极材料用双层结构匣钵，其特征在于，所述外层的厚度为10～15mm，内层的厚度为2-3mm。
3.根据权利要求1或2所述一种锂电池正极材料用双层结构匣钵，其特征在于，所述锂电池正极材料用双层结构匣钵的气孔率为15-30％。
4.根据权利要求1或2所述一种锂电池正极材料用双层结构匣钵，其特征在于，所述锂电池正极材料用双层结构匣钵的抗压强170-220MPa。
5.根据权利要求1或2所述一种锂电池正极材料用双层结构匣钵，其特征在于，所述锂电池正极材料用双层结构匣钵的堆积密度2.5-4.5g/cm3。
6.一种锂电池正极材料用双层结构匣钵的制备方法，其特征在于，采用权利要求1或2所述一种锂电池正极材料用双层结构匣钵的原料，其制备方法包括如下步骤：
S1外层混料：将堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照外层物料配方比例进行筛选、称量并混合均匀；
S2外层成型：将混合好的原料放入陶瓷匣钵的预模具中进行成型，制成匣钵生坯；
S3内层混合制浆：将内层的纳米氧化锆、堇青石、莫来石、美铝尖晶石、氧化铝、高岭土和硼酸盐玻璃按照内层物料配方比例称量并加入20-40份水混合均匀，制成浆料；
S4内层制备，将浆料采用喷涂机涂布在所述匣钵生坯的内表面，再放入成品模具中进行成型，成型后，盖上密封盖，对成型模具内部进行抽真空并加压成型，然后进行干燥处理；
S5烧成：经过干燥后的匣钵放入烧成炉中进行烧成处理， 获得锂电池正极材料用双层结构匣钵。
7.根据权利要求6所述一种锂电池正极材料用双层结构匣钵的制备方法，其特征在于，在步骤S4成型中，所述抽真空的真空度为800-1000Pa。
8.根据权利要求6所述一种锂电池正极材料用双层结构匣钵的制备方法，其特征在于，在步骤S4成型中，所述加压成型压力为400-600kgf/cm2并保压12h-14h。
9.根据权利要求6所述一种锂电池正极材料用双层结构匣钵的制备方法，其特征在于，在步骤S5烧结中，所述烧结温度为1200-1300℃，烧成时间为2-4小时。
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