CN111424267B - 一种制备镍包覆铋硫氯的方法 - Google Patents
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Abstract
本发明公开了一种制备镍包覆铋硫氯的方法,属于材料制备技术领域。本发明所述方法通过液相辅助溶剂热还原法在铋硫氯晶粒表面包覆一层镍单质。方法包括:铋硫氯粉体研磨、稀盐酸浸泡清洗除杂;超声震荡分散;浸泡氢氧化钠溶液10~20min;加入硫酸镍溶液使表面形成氢氧化镍颗粒包覆;使用液相辅助溶剂热还原法还原氢氧化镍;离心、洗涤、干燥得到晶粒表面均匀包覆镍单质的包镍铋硫氯材料。本发明所述方法工艺简单,设备要求低,通过包覆镍修饰铋硫氯晶粒表面,维持铋硫氯自身较高的初始塞贝克系数,电导率性能得到了极大的改善。
Description
技术领域
本发明涉及一种制备镍包覆铋硫氯的方法,属于材料制备技术领域。
背景技术
三元铋硫属化合物自发现以来,因其自身独特的带隙可控性质、优异的光电以及热电性能参数,在许多领域特别是在半导体电能转换领域存在着巨大的潜力。例如BiSX,BiOCl和CdZnTe已广泛用于光催化和光伏电池。经调查表明,属于本体系的铋硫氯材料大多具有1.7-2.0eV的带隙,在可见光波段具有较强的吸光系数,极高的塞贝克系数以及较低的热导率。但是由于其自身的晶格结构所限,铋硫氯材料表现出极低的电导率性质,因此极大程度的影响了其在半导体电学转换方面的应用。
毋庸置疑,提高铋硫氯的导电性会对此材料带来性能方面的巨大提升。对于提高电导率的方法,一方面可以通过掺杂其他元素,提升其载流子浓度来增强材料的导电性;另一方面可以通过化学镀的方式在其晶粒表面包覆一层导电性高的材料辅助提升材料的导电性。众所周知,镍具有良好的导电性,化学镀镍是一种成熟的工艺,可以将镍元素均匀地沉积在材料的晶粒表面。在铋硫氯晶体表面镀镍是一种可行的方案。
目前尚未有在铋硫氯表面镀镍的报道,同时经调查目前在其他材料表面镀镍的方法多使用水合肼计较高的镀镍温度,镀镍过程存在一定的危害。
发明内容
本发明的目的在于针对上述现有技术的不足,提供一种制备镍包覆铋硫氯的方法;本方法摒弃了水合肼的使用,通过溶液法对铋硫氯进行化学镀镍;所制备的粉体为以铋硫氯为核、以镍单质为壳的核壳结构,可用于对铋硫氯电导率的优化;本发明通过以下技术实现。
(1)按比例称取铋硫氯粉体,经研磨粉碎转入盐酸溶液超声酸洗,然后蒸馏水超声洗涤,离心分离,得到分散的铋硫氯粉体。
(2)将步骤(1)所得分散的铋硫氯粉体加入至氢氧化钠溶液中(此处氢氧化钠溶液的量全部浸泡铋硫氯粉体即可,优选固液比为1:15),粉末完全浸泡在氢氧化钠溶液中,浸泡超声10~20min,过滤,制得表面附有氢氧化钠的铋硫氯前驱体。
(3)将步骤(2)所得的前驱体铋硫氯转入至搅拌条件下的镍盐溶液中,加热20~30min,过滤分离,制得表面附有氢氧化镍纳米颗粒的铋硫氯晶体。
(4)将步骤(3)所得表面附有氢氧化镍纳米颗粒的铋硫氯粉体转入至还原剂溶液中,搅拌条件下,加热、保温5~7h;自然冷却至室温,经离心、洗涤、干燥后得到镍包覆铋硫氯材料;其中,粉体与还原剂溶液比例为15~20g/L。
优选的,本发明步骤(1)中所述的稀盐酸溶液其浓度为2~4%;超声酸洗时间为5~7min;蒸馏水超声洗涤时间为30-40min。
优选的,本发明步骤(2)所使用氢氧化钠(NaOH)溶液的浓度为15~18g/L。
优选的,本发明步骤(3)所使用的镍盐为六水硫酸镍(NiSO4·6H2O),镍盐溶液的浓度为25~30g/L;搅拌过程中的转速为270-400r/min;加热温度为65~85℃。
优选的,本发明步骤(4)中所还原剂溶液成分:三亚乙基四胺(TETA,纯度为70%)、乙二醇(EG,纯度为99%),体积比9:1~8.5:1.5;加热温度为110-130℃。
本发明的有益效果:
(1)与现有的在其他材料表面镀镍方法相比较,本方法所摒弃了有毒的水合肼的使用,药剂安全无污染。
(2)使用硫酸镍与氢氧化钠反应,生成的氢氧化镍纳米颗粒为纳米线形状,易在表被包覆者晶体面形成缠绕层,包覆不易脱落;使用弱还原剂TETA,体系粘度较大,减少了团聚现象,还原的单质镍晶粒更加均匀,镍包覆层更加致密均匀。
(3)镍包覆层较薄,对材料自身其他性质影响较小,同时可以根据在硫酸镍中的反应时间长短来控制氢氧化钠包覆层的厚度,进而控制镍包覆层的厚度。
附图说明
图1为原始样品的SEM图;
图2为实施例1制备的样品的SEM图;
图3为实施例1制备的样品的XRD图;
图4为镍包覆铋硫氯(Ni@BiSCl)与未包覆镍的原始铋硫氯(BiSCl)的导电性能比较图。
具体实施方式
下面结合具体实施例本发明作进一步的详细说明,但本发明的保护范围并比限于所述内容。
实施例1
一种制备镍包覆铋硫氯的方法,其具体步骤包括:
(1)将2g铋硫氯粉末至于30ml浓度为3%的稀盐酸盐酸溶液中,超声5min后离心分离稀盐酸溶液,并用蒸馏水超声30min,用蒸馏水洗涤至中性并干燥。
(2)配置30ml浓度为16g/L的氢氧化钠溶液,放入2g步骤1所得的粉末,超声震荡15min;过滤分离氢氧化钠溶液。
(3)将步骤(2)制得的表面附有氢氧化钠基团的铋硫氯粉末缓慢置入搅拌条件下100ml溶有2.6g六水硫酸镍溶液中,升温至80℃,保温30min;过滤分离出固体颗粒,得到表面包覆有氢氧化镍纳米颗粒的铋硫氯粉体。
(4)使用三颈瓶,加入90ml三亚乙基四胺、10ml乙二醇溶液,加入步骤3所得表面附有氢氧化镍颗粒的铋硫氯粉体;安装回流冷凝管,搅拌条件下升温至120℃,保温5h。自然冷却至室温,使用乙醇进行离心洗涤3次,干燥,得到黑色粉末颗粒,即为外层均匀包覆镍单质的铋硫氯粉体。
本实施例所制备的镍包覆铋硫氯粉体晶形貌如图2所示,与图1原始状态相对比,可以看出在铋硫氯晶体表面均匀包覆有微小颗粒;图3显示所制备的粉体中有镍单质存在,无其他杂质,表明包覆物质为镍单质。图4可以看出,经过镍包覆的铋硫氯粉体的电导率与未包覆的粉体相比较,由于表层的镍单质构成到导电通道,电导率有明显的提高,在500K温度下,电导率由原始的0.013S/cm提升至0.494S/cm。
实施例2
一种制备镍包覆铋硫氯的方法,其具体步骤包括:
(1)将2g铋硫氯粉末至于30ml浓度为2%的稀盐酸盐酸溶液中,超声6min后离心分离稀盐酸溶液,并用蒸馏水超声35min,用蒸馏水洗涤至中性并干燥。
(2)配置30ml浓度为15g/L的氢氧化钠溶液,放入2g步骤1所得的粉末,超声震荡10min;过滤分离氢氧化钠溶液。
(3)将步骤(2)制得的表面附有氢氧化钠基团的铋硫氯粉末缓慢置入搅拌条件下100ml溶有3.0g六水硫酸镍溶液中,升温至65℃,保温25min;过滤分离出固体颗粒,得到表面包覆有氢氧化镍纳米颗粒的铋硫氯粉体。
(4)使用三颈瓶,加入85ml三亚乙基四胺、15ml乙二醇溶液,加入步骤3所得表面附有氢氧化镍颗粒的铋硫氯粉体;安装回流冷凝管,搅拌条件下升温至120℃,保温5h。自然冷却至室温,使用乙醇进行离心洗涤3次,干燥,得到黑色粉末颗粒,即为外层均匀包覆镍单质的铋硫氯粉体。
本实施例所制备的镍包覆铋硫氯粉体晶形貌与实施例1相似,在铋硫氯晶体表面均匀包覆有微小颗粒;制备的粉体中有镍单质存在,无其他杂质,表明包覆物质为镍单质。经过镍包覆的铋硫氯粉体的电导率与未包覆的粉体相比较,电导率有明显的提高,在500K温度下,电导率由原始的0.013S/cm提升至0.487S/cm。
实施例3
一种制备镍包覆铋硫氯的方法,其具体步骤包括:
(1)将2g铋硫氯粉末至于30ml浓度为4%的稀盐酸盐酸溶液中,超声7min后离心分离稀盐酸溶液,并用蒸馏水超声40min,用蒸馏水洗涤至中性并干燥。
(2)配置30ml浓度为18g/L的氢氧化钠溶液,放入2g步骤1所得的粉末,超声震荡20min;过滤分离氢氧化钠溶液。
(3)将步骤(2)制得的表面附有氢氧化钠基团的铋硫氯粉末缓慢置入搅拌条件下100ml溶有2.8g六水硫酸镍溶液中,升温至85℃,保温20min;过滤分离出固体颗粒,得到表面包覆有氢氧化镍纳米颗粒的铋硫氯粉体。
(4)使用三颈瓶,加入87ml三亚乙基四胺、13ml乙二醇溶液,加入步骤3所得表面附有氢氧化镍颗粒的铋硫氯粉体;安装回流冷凝管,搅拌条件下升温至120℃,保温5h;自然冷却至室温,使用乙醇进行离心洗涤3次,干燥,得到黑色粉末颗粒,即为外层均匀包覆镍单质的铋硫氯粉体。
本实施例所制备的镍包覆铋硫氯粉体晶形貌与实施例1相似,在铋硫氯晶体表面均匀包覆有微小颗粒;制备的粉体中有镍单质存在,无其他杂质,表明包覆物质为镍单质。经过镍包覆的铋硫氯粉体的电导率与未包覆的粉体相比较,电导率有明显的提高,在500K温度下,电导率由原始的0.013S/cm提升至0.491S/cm。
Claims (4)
1.一种制备镍包覆铋硫氯的方法,其特征在于,具体包含以下步骤:
(1)按比例称取铋硫氯粉体,经研磨粉碎转入盐酸溶液超声酸洗,然后蒸馏水超声洗涤,离心分离,得到分散的铋硫氯粉体;
(2)将步骤(1)所得分散的铋硫氯粉体加入至氢氧化钠溶液中,粉末完全浸泡在氢氧化钠溶液中,浸泡超声10~20min,过滤,制得表面附有氢氧化钠的铋硫氯前驱体;
(3)将步骤(2)所得的前驱体铋硫氯转入至搅拌条件下的镍盐溶液中,加热20~30min,过滤分离,制得表面附有氢氧化镍纳米颗粒的铋硫氯晶体;
(4)将步骤(3)所得表面附有氢氧化镍纳米颗粒的铋硫氯粉体转入至还原剂溶液中,搅拌条件下,加热、保温5~7 h;自然冷却至室温,经离心、洗涤、干燥后得到镍包覆铋硫氯材料;其中,粉体与还原剂溶液比例为15~20 g/L;
步骤(3)所使用的镍盐为六水硫酸镍(NiSO4•6H2O),镍盐溶液的浓度为25~30 g/L,加热温度为65~85℃;
步骤(4)中所还原剂溶液成分:三亚乙基四胺、乙二醇,体积比9:1~8.5:1.5;加热温度为110-130℃。
2.根据权利要求1所述制备镍包覆铋硫氯的方法,其特征在于:步骤(1)中所述稀盐酸溶液其浓度为2~4%;超声酸洗时间为5~7min;蒸馏水超声洗涤时间为30-40min。
3.根据权利要求1所述制备镍包覆铋硫氯的方法,其特征在于:步骤(2)所使用氢氧化钠(NaOH)溶液的浓度为15~18g/L。
4.根据权利要求1所述制备镍包覆铋硫氯的方法,其特征在于:步骤(3)中搅拌过程的转速为270-400 r/min。
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