CN116409785A - 一种球化石墨尾料负极材料及其加工方法 - Google Patents
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Abstract
一种球化石墨尾料负极材料及其加工方法,方法包括以下步骤:(1)将粘结剂和球型石墨尾料加入到混合机中混合,得到第一前驱体;(2)将第一前驱体压粉并填充到等静压成型机中,加压成块,将块状物打散磨粉,得到第二前驱体;(3)将第二前驱体,经石墨化、解聚打散后,得到第三前驱体;(4)将第三前驱体进行气相碳源包覆,包覆碳层厚度10‑20nm,得到球化石墨尾料负极材料。石墨球型尾料本身是小粒径材料,经造粒后为小粒径复合结构,比表面积较小,因此再引入天然气褶皱碳层结构,可促使材料倍率性能进一步提升。
Description
技术领域
本发明属于锂离子电池负极技术领域,尤其涉及一种球化石墨尾料负极材料及其加工方法。
背景技术
最近随着电子便携设备和电动汽车的发展,对石墨材料需求逐渐增加,但在天然石墨球化过程中,会产生40%左右的细粉尾料,现有尾料的存在粒度小、比表大、杂质含量高、振实密度低、压实低等问题,由于处理工艺相对复杂,应用价值较低,基本处于废置状态。现有技术中,多为对石墨尾料直接进行球形化、混合粘结剂、混压、焙烧、破碎处理得到负极材料,但未能解决石墨尾料本身为细粉结构,造粒粒度小,获得的材料倍率性能较低的缺陷。
发明内容
本发明所要解决的技术问题是天然石墨球化过程中产生的细粉尾料的回收,克服以上背景技术中提到的不足和缺陷,提供一种球化石墨尾料负极材料及其加工方法。
为解决上述技术问题,本发明提出的技术方案为:
一种球化石墨尾料加工方法,包括以下步骤:
(1)将粘结剂和球型石墨尾料加入到混合机中混合,得到第一前驱体;
(2)将第一前驱体压粉并填充到等静压成型机中,加压成块,将块状物打散磨粉,得到第二前驱体;
(3)将第二前驱体,经石墨化、解聚打散后,得到第三前驱体;
(4)将第三前驱体进行气相碳源包覆,包覆碳层厚度10-20nm,得到球化石墨尾料负极材料。
常规有机气源有乙烯、乙炔、沥青等固体碳源,而天然气形成的包覆碳层,为褶皱独有结构,且结构强度较其它碳层更好。
在石墨化后使用天然气气相碳源包覆,会形成表面褶皱类型碳层形貌,电池充放电过程,褶皱碳层,锂离子更容易从褶皱间隙嵌入到石墨碳层内部,有更多嵌入位点;而传统平整碳层,只能通过碳层层空隙位点嵌入到石墨碳层内部,位点较少。采用天然气气相碳源包覆,会形成褶皱碳层,褶皱碳层之间存在纳米级别间隙,锂离子可以从间隙为向内层及石墨扩散,能够更好地将锂离子引入小粒径石墨碳层中,大幅度提升材料的性质。
优选的,所述石墨尾料为天然石墨球化过程中产生的尾料,D50为3-6μm,振实密度0.40-0.50g/cm3。
天然石墨尾料D50很低,直接进行石墨化和球化处理后得到的球化颗粒同样为小粒径复合结构,作为负极材料,倍率性能仍旧具有很大提升空间。
优选的,所述粘结剂为沥青或树脂粘结剂,所述粘结剂和球型石墨尾料的质量比为90%-70%:10%-30%。
优选的,所述石墨化时间为4-24h。
优选的,所述气相碳源为天然气。
在同一个技术构思下,本发明还提供一种球化石墨尾料加工方法制备得到的球化石墨尾料负极材料,所述负极材料为核壳式结构,内层为球型石墨尾料与粘结剂复合结构,碳层均匀包覆在表面,厚度为10-20nm。
优选的,所述球化石墨尾料负极材料D50为12-18μm,振实密度0.70-0.8g/cm3。
与现有技术相比,本发明的有益效果为:
(1)充分再利用天然石墨球化尾料,可通过混合粘结剂+等静压+磨粉+石墨化,使用有机气源对处理物料进行包覆,天然气气源包覆碳层,有利于材料倍率性能提升,使球型石墨尾料达到可利用水平,具有环保回收意义。
(2)石墨球型尾料本身是小粒径材料,经造粒后为小粒径复合结构,比表面积较小,因此再引入天然气褶皱碳层结构,可促使材料倍率性能进一步提升。
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为实施例1中球化石墨尾料负极材料的天然气包覆碳层形貌图;
图2为对比例1中球化石墨尾料负极材料的沥青包覆碳层形貌图。
具体实施方式
为了便于理解本发明,下文将结合较佳的实施例对本发明做更全面、细致地描述,但本发明的保护范围并不限于以下具体实施例。
除非另有定义,下文中所使用的所有专业术语与本领域技术人员通常理解含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的,并不是旨在限制本发明的保护范围。
除非另有特别说明,本发明中用到的各种原材料、试剂、仪器和设备等均可通过市场购买得到或者可通过现有方法制备得到。
实施例1:
将球型石墨尾料与软化点150℃沥青按80%:20%质量比例混合,采用等静压工艺,将混合物料压制成型,通过磨粉方法可得到D50在12-15μm的物料,物料经3000℃-6h石墨化,经解聚打散,以天然气为有机气源,在1000℃进行气相包覆2h,包覆碳层设计10-20nm,得到实施例1的一种球化石墨尾料加工方法制备得到的球化石墨尾料负极材料。
负极材料为核壳式结构,内层为球型石墨尾料与粘结剂复合结构,天然气碳层均匀包覆在表面,厚度为10-20nm。如图1所示,天然气包覆碳层表面为褶皱形貌。球化石墨尾料负极材料D50为13μm,振实密度0.72g/cm3。
实施例2:
将球型石墨尾料软化点150℃沥青按70%:30%质量比例混合,采用等静压工艺,将混合物料压制成型,通过磨粉方法可得到D50在12-15μm的物料,物料经3000℃-6h石墨化,经解聚打散,以天然气为有机气源,在1000℃进行气相包覆2h,包覆碳层设计10-20nm,得到实施例的一种球化石墨尾料加工方法制备得到的球化石墨尾料负极材料。
负极材料为核壳式结构,内层为球型石墨尾料复合结构,碳层均匀包覆在表面,厚度为10-20nm。球化石墨尾料负极材料D50为14μm,振实密度0.73g/cm3。
对比例1:
将球型石墨尾料软化点150℃沥青按70%:30%质量比例混合,采用等静压工艺,将混合物料压制成型,通过磨粉方法可得到D50在12-15μm的物料,物料经3000℃-6h石墨化,经解聚打散,加入5%沥青混合均匀,在1000℃进行碳化处理,沥青包覆层厚度10-20nm,得到对比例负极材料。如图2所示,沥青包覆碳层表面为较为平整形貌。
实施例和对比例所制备的负极材料的电化学测试结果如表所示。
表1:本发明的实施例与对比例得到的为电性能对比结果。
从表1可以看出,采用本发明的方法可以将天然石墨球型尾料(如D50为3-6μm)制备成可利用负极材料,球型石墨尾料无法在电池加工过程直接应用,通过本发明制备工艺方法,具有较高的实用性,相对于沥青混合包覆,天然气CVD包覆后,由于天然气表面碳层具备褶皱形貌结构,拥有更多的锂离子嵌入通道,因此材料倍率性能更优。
Claims (7)
1.一种球化石墨尾料加工方法,其特征在于,包括以下步骤:
(1)将粘结剂和球型石墨尾料加入到混合机中混合,得到第一前驱体;
(2)将第一前驱体压粉并填充到等静压成型机中,加压成块,将块状物打散磨粉,得到第二前驱体;
(3)将第二前驱体,经石墨化、解聚打散后,得到第三前驱体;
(4)将第三前驱体进行气相碳源包覆,包覆碳层厚度10-20nm,得到球化石墨尾料负极材料。
2.如权利要求1所述的球化石墨尾料加工方法,其特征在于,所述石墨尾料为天然石墨球化过程中产生的尾料,D50为3-6μm,振实密度0.40-0.50g/cm3。
3.如权利要求1所述的球化石墨尾料加工方法,其特征在于,所述粘结剂为沥青或树脂粘结剂,所述粘结剂和球型石墨尾料的质量比为(90-70):(10-30)。
4.如权利要求1所述的球化石墨尾料加工方法,其特征在于,所述石墨化时间为4-24h。
5.如权利要求1所述的球化石墨尾料加工方法,其特征在于,所述气相碳源为天然气。
6.一种如权利要求1-5任一项所述球化石墨尾料加工方法制备得到的球化石墨尾料负极材料,其特征在于,所述负极材料为核壳式结构,内层为球型石墨尾料与粘结剂复合结构,褶皱状碳层均匀包覆在表面,厚度为10-20nm。
7.如权利要求6所述的球化石墨尾料负极材料,其特征在于,所述球化石墨尾料负极材料D50为12-18μm,振实密度0.70-0.80g/cm3。
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CN117682515B (zh) * | 2023-11-22 | 2024-05-31 | 云南锂宸新材料科技有限公司 | 一种二次造粒天然石墨的制备方法及其产品和应用 |
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CN117682515B (zh) * | 2023-11-22 | 2024-05-31 | 云南锂宸新材料科技有限公司 | 一种二次造粒天然石墨的制备方法及其产品和应用 |
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