CN115124007A - 一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法 - Google Patents
一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种多级调控亲水性‑疏水性硼碳氮纳米材料的制备方法。以硼酸和三聚氰胺等原料,氯化钾与氧化铜金属氧化物为助剂,惰性气氛下进行热处理及酸处理,制得硼碳氮纳米材料。该方法通过调节助剂氧化铜的用量以及热处理时间,可实现硼碳氮纳米材料亲疏水性能的多级调变。制备得到亲水性的纳米颗粒和纳米片层材料,以及疏水性的纳米颗粒和纳米片层材料。制备工艺安全简便,材料的可应用范围广。本发明尤其是提供了一种超疏水性硼碳氮纳米材料及其制备方法,对于硼碳氮纳米材料的多领域应用具有实际价值。
Description
技术领域
本发明属于纳米材料制备技术领域,涉及一种可用于不同亲疏水性能的硼碳氮纳米材料的调控制备方法。
背景技术
近年来,纳米结构材料在表面非润湿性方面开辟了一个新纪元,并激发了人们对其在自清洁表面、保护涂层、防雾玻璃和耐污材料等潜在应用的极大兴趣。其中,硼、碳、氮三种相邻的轻元素所形成的新材料受到了大家的广泛关注。石墨烯被发现以来,其优异的导电性能、机械性能、光学性能等得到了认可和应用;作为等电子体的氮化硼因其良好的介电性、导热性、化学惰性、耐磨性等特性而备受关注;而硼碳氮三元化合物材料兼具碳材料以及氮化硼两者的优点,是介于导电材料和介电材料的半导体材料。制备硼碳氮材料的方法有多种,包括化学沉积法、水热法、磁控溅射法、高温煅烧法等。已有报道大多数是有关亲水性的硼碳氮材料(张云启,高比表硼碳氮纳米片的制备及其吸附性能研究[D],2019);而疏水性的硼碳氮材料研究较少,一般是通过引入疏水有机物与其复合而形成疏水性的硼碳氮复合材料(Bharathidasan T et al.ACS Applied Materials&Interfaces,2015,7(33):18450-9);自身具有疏水性的硼碳氮材料鲜有报道。为了对疏水性硼碳氮材料的开发和利用提供基础,本发明提出了一种可制备超疏水性硼碳氮纳米材料的方法,尤其是可实现多级调控亲水性-疏水性硼碳氮材料的形成。本发明通过简单地调节助剂用量和反应热处理时间,可得到由亲水性到超疏水性变化的不同硼碳氮纳米材料,制备过程简便可控。
发明内容
为获得具有超疏水特性的硼碳氮材料,本发明提供了一种简单易行的热分解法调控制备硼碳氮纳米材料的方法,实现多级调节硼碳氮纳米材料的亲疏水性,得到一系列不同亲疏水性能的硼碳氮纳米材料。
本发明所提供的制备方法,采用如下技术方案:
一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法,其特征在于,包括以下步骤:
将反应物硼酸、三聚氰胺和助剂氯化钾、金属氧化物研磨混合,置于管式炉中,在惰性气氛保护下,以一定温度进行高温热处理一段时间后,取出所得固体产物并用酸处理,离心去除上清液,用去离子水多次离心洗涤,干燥,得到粉末状固体产物为硼碳氮纳米材料。制备方法主要有以下特征:
通过调节助剂金属氧化物的含量和高温反应的热处理时间,实现对硼碳氮材料的亲疏水性能多级调控。
硼酸和三聚氰胺用量的摩尔比为0.5:1~5:1。
氯化钾和硼酸用量的摩尔比为0.2:1~5:1。
金属氧化物和硼酸用量的摩尔比为0:1~5:1。
助剂金属氧化物为氧化铜、氧化钴、氧化锌、氧化铁、氧化镍以及其他常用的金属氧化物中的一种或多种。
惰性气体为氮气、氩气、氦气中的一种。酸处理用的酸为盐酸、硝酸中的一种。
硼碳氮纳米材料包括粒径为20~150nm的球形纳米颗粒,尺寸为0.5~200μm的纳米薄片层材料。
载气流速为50~120mL/min;高温煅烧温度为800~1200℃;煅烧时间为2~10小时。
硼碳氮纳米材料包括BC2N、B2CN及其他不同B、C、N含量组成的硼碳氮三元化合物中的一种或多种。
不同于其他的制备方法,本发明的方法所制备得到的硼碳氮材料为从接触角低至30°的亲水性硼碳氮材料,接触角逐渐增大的硼碳氮材料,以至接触角高达150°的超疏水性硼碳氮材料。本发明提供了可控调节硼碳氮纳米材料形成的方法,可得到不同亲疏水性能的多种硼碳氮材料,尤其是能直接制备得到自身超疏水性的硼碳氮纳米材料,该材料具有潜在的市场应用价值。
附图说明:
图1为本发明实例制得硼碳氮材料的SEM图;
图2为本发明实例制得硼碳氮材料的接触角测试图。
具体实施方式
下面结合实施例对本发明作进一步说明,但本发明并不限于以下实施例。
实施例1
取20mmol硼酸、10mmol三聚氰胺、60mmol氯化钾混合研磨后,转移至管式炉中;在气速为100mL·min-1的氮气氛下升温加热,160℃预热50min后,程序升温至950℃反应时间4h。将获得的固体物用稀盐酸浸泡,离心,去离子水多次洗涤后,将沉淀物于60℃的鼓风干燥箱中干燥12h,得到白色产物即为亲水性的硼碳氮纳米片。
实施例2
取20mmol硼酸、10mmol三聚氰胺、60mmol氯化钾及40mmol氧化钴混合研磨后,转移至管式炉中;在气速为100mL·min-1的氮气氛下升温加热,160℃预热50min后,程序升温至950℃反应时间4h。将获得的固体物用稀盐酸浸泡,离心,去离子水多次洗涤后,将沉淀物于60℃的鼓风干燥箱中干燥12h,得到白色产物即为亲水性的硼碳氮纳米颗粒。
实施例3
取20mmol硼酸、10mmol三聚氰胺、60mmol氯化钾及60mmol氧化铜混合研磨后,转移至管式炉中;在气速为80mL·min-1的氮气氛下升温加热,160℃预热50min后,程序升温至1000℃反应时间4h。将获得的固体物用稀盐酸浸泡,离心,去离子水多次洗涤后,将沉淀物于60℃的鼓风干燥箱中干燥12h,得到白色产物即为疏水性的硼碳氮纳米片材料。
实施例4
取20mmol硼酸、10mmol三聚氰胺、60mmol氯化钾及60mmol氧化铜混合研磨后,转移至管式炉中;在气速为80mL·min-1的氮气氛下升温加热,160℃预热50min后,程序升温至950℃反应时间6h。将获得的固体物用稀盐酸浸泡,离心,去离子水多次洗涤后,将沉淀物于60℃的鼓风干燥箱中干燥12h,得到白色产物即为疏水性的硼碳氮纳米片材料。
Claims (8)
1.一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法,其特征在于,包括以下步骤:将反应物硼酸、三聚氰胺和助剂氯化钾、金属氧化物按一定的比例混合,研磨均匀,将混合粉末置于管式炉内;在一定流速的惰性气氛保护下,混合物经预热处理,并在设定的温度下进行高温热解反应,控制一定的反应时间,自然降温,得到固态产物;将上述固态产物取出,经稀酸处理,离心,去离子水多次洗涤,干燥,得到粉末状固体产物,即为硼碳氮纳米材料。
2.按照权利要求1所述的一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法,其特征在于,通过助剂金属氧化物含量和高温反应热处理时间的协同调节,实现对硼碳氮材料的亲疏水性能的多级调控。
3.按照权利要求1所述的一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法,其特征在于,硼碳氮纳米材料包括BC2N、B2CN及其他不同B、C、N含量组成的硼碳氮三元化合物中的一种或多种。
4.按照权利要求1所述的一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法,其特征在于,硼碳氮纳米材料包括粒径为20~150nm的球形纳米颗粒以及尺寸为0.5~200μm的纳米薄片层材料。
5.按照权利要求1所述的一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法,其特征在于,硼酸和三聚氰胺用量的摩尔比为0.5:1~5:1。氯化钾和硼酸用量的摩尔比为0.2:1~5:1。
6.按照权利要求1所述的一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法,其特征在于,助剂金属氧化物为氧化铜、氧化钴、氧化锌、氧化铁、氧化镍以及其他常用的金属氧化物中的一种或多种。金属氧化物和硼酸用量的摩尔比为0:1~5:1。
7.按照权利要求1所述的一种多级调控亲水性-疏水性硼碳氮纳米材料的制备方法,其特征在于,载气流速为50~120mL/min;高温煅烧温度为800~1200℃;煅烧时间为2~10小时;惰性气体为氮气、氩气、氦气中的一种。酸处理用的酸为盐酸、硝酸中的一种。
8.按照权利要求1-7任一项所述方法制备亲水性-疏水性硼碳氮纳米材料,其特征在于,可以调控制得从低接触角低至30°的亲水性硼碳氮材料,接触角逐渐增大的硼碳氮材料,以至接触角高达150°超疏水性的多种硼碳氮材料。
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