CN110950350A - 一种室温制备二硼化钪纳米粒子的方法 - Google Patents
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Abstract
本发明公开了一种室温制备二硼化钪纳米粒子的方法。本发明通过液相等离子体,在室温于1‑丁基‑3‑甲基咪唑硫氰酸盐离子液体中,通过硼烷还原ScCl3合成出二硼化钪纳米粒子。与商用二硼化钪相比,本发明所制备的二硼化钪纳米粒子比表面积更大,抑菌效果更强。与丁胺卡那霉素和硫酸威替米星相比,本发明所制备的二硼化钪纳米粒子对雷氏普罗威登斯菌表现出了更强的抗菌活性。其优异的雷氏普罗威登斯菌抑菌功能使二硼化钪有望在烧伤、创伤和尿道感染等临床治疗领域方面得到广泛应用。
Description
技术领域
本发明涉及一种室温制备二硼化钪纳米粒子的方法,属于先进纳米材料制备技术领域。
背景技术
二硼化钪是一种半导体,轻质耐火及耐磨材料,一般通过高温烧结的方法来制备,不仅耗能,而且耗时。所以,非常有必要拓展新的绿色合成方法或技术途径来制备二硼化钪。
发明内容
本发明通过液相等离子体技术,首次在室温于1-丁基-3-甲基咪唑硫氰酸盐离子液体中通过硼烷还原ScCl3合成出二硼化钪纳米粒子,其具平均粒径为4.4nm左右,同时具有较优的雷氏普罗威登斯菌抑菌活性。雷氏普罗威登斯菌在一定条件下能引起各种感染,已成为重要的医源性感染条件致病菌,可引起烧伤、创伤和尿道感染等。
本发明采用如下技术方案:
本发明的二硼化钪纳米粒子的制备方法的具体步骤如下:
(1)将1.8mmol ScCl3加入24mL1-丁基-3-甲基咪唑硫氰酸盐离子液体中,在氩气保护下搅拌17分钟,以形成溶液;
(2)在氩气保护下把步骤(1)的混合液中转入50mL反应釜,通入硼烷,使硼烷与ScCl3的摩尔比为3.5-6.5:1,密闭反应釜;
(3)开启液相等离子体,功率为450-750W,对步骤(2)反应釜中的混合溶液在室温下进行处理25-55min后得到二硼化钪纳米粒子粗品;
(4)将产物用去离子水洗涤三次,再用无水乙醇洗涤三次,干燥备用。
步骤(2)中,优选在氩气保护和硼烷与ScCl3的摩尔比为5:1往步骤(1)的混合液中通入硼烷,密闭反应釜。
步骤(3)中,优选液相等离子体的功率为600W。
步骤(3)中,优选反应时间为40min。
本发明的积极效果如下:
1)本发明通过采用液相等离子体技术,首次成功地在室温下合成出二硼化钪纳米粒子。
2)与商用二硼化钪对比,本发明合成的二硼化钪纳米粒子的比表面积更大。
3)与商用二硼化钪对比,本发明合成的二硼化钪纳米粒子表现出更强的抗菌活性。
4)与丁胺卡那霉素和硫酸威替米星相比,本发明合成的二硼化钪纳米粒子对雷氏普罗威登斯菌表现出更强的抗菌活性。
附图说明
图1是实施例1所制备二硼化钪纳米粒子的TEM照片。
图2是实施例1所制备二硼化钪纳米粒子的X射线衍射图谱。
图3是实施例1所制备二硼化钪纳米粒子的Sc2pXPS图谱。
图4是实施例1所制备二硼化钪纳米粒子的B1sXPS图谱。
具体实施方式
下面的实施例是对本发明的进一步详细描述。
下述实施例中所使用的实验方法如无特殊说明,均为常规方法。
下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1
(1)将1.8mmol ScCl3加入24mL1-丁基-3-甲基咪唑硫氰酸盐离子液体中,在氩气保护下搅拌17分钟,以形成溶液;
(2)在氩气保护下把步骤(1)的混合液中转入50mL反应釜,通入硼烷,使硼烷与ScCl3的摩尔比为5:1,密闭反应釜;
(3)开启液相等离子体,功率为600W,对步骤(2)反应釜中的混合溶液在室温下进行处理40min后得到二硼化钪纳米粒子粗品;
(4)将产物用去离子水洗涤三次,再用无水乙醇洗涤三次,干燥备用。
实施例2
(1)将1.8mmol ScCl3加入24mL1-丁基-3-甲基咪唑硫氰酸盐离子液体中,在氩气保护下搅拌17分钟,以形成溶液;
(2)在氩气保护下把步骤(1)的混合液中转入50mL反应釜,通入硼烷,使硼烷与ScCl3的摩尔比为5:1,密闭反应釜;
(3)开启液相等离子体,功率为450W,对步骤(2)反应釜中的混合溶液在室温下进行处理40min后得到二硼化钪纳米粒子粗品;
(4)将产物用去离子水洗涤三次,再用无水乙醇洗涤三次,干燥备用。
实施例3
(1)将1.8mmol ScCl3加入24mL1-丁基-3-甲基咪唑硫氰酸盐离子液体中,在氩气保护下搅拌17分钟,以形成溶液;
(2)在氩气保护下把步骤(1)的混合液中转入50mL反应釜,通入硼烷,使硼烷与ScCl3的摩尔比为5:1,密闭反应釜;
(3)开启液相等离子体,功率为750W,对步骤(2)反应釜中的混合溶液在室温下进行处理40min后得到二硼化钪纳米粒子粗品;
(4)将产物用去离子水洗涤三次,再用无水乙醇洗涤三次,干燥备用。
本发明的二硼化钪纳米粒子的性能:
采用TEM对实施例1所制备样品进行了表征,图1为样品的TEM图像。从图1可以看出,样品的平均粒径为4.4nm左右。
采用XRD对样品的物相组成进行了分析。从图谱中(图2)可以看出,样品没有明显的特征衍射峰,说明其具有非晶性质。此外,样品的Sc2pXPS图谱(图3)和B1sXPS图谱(图4)表明形成了二硼化钪纳米粒子合金。
ICP-AES分析测试结果表明,所制备的二硼化钪纳米粒子与商用二硼化钪的元素质量百分组成相同(Sc:67.52;B:32.48)。实施例1所制备二硼化钪纳米粒子的比表面积为128.4m2g-1,远大于商用二硼化钪(11.1m2g-1)。
对所制备二硼化钪纳米粒子的抗菌活性进行了研究(表1)。通过比色法测定抑菌浓度(MICs,μgmL-1)的方法,来确定样品对甲氧西林敏感金葡菌(S.aureus),表皮葡萄球菌(S.epidermidis),鲍曼不动杆菌(A.baumanii),类鼻疽假单胞菌(P.pseudomallei)和雷氏普罗威登斯菌(P.rettgeri)的抗菌活性。作为比较,商用二硼化钪,丁胺卡那霉素和硫酸威替米星的抗菌活性也列于表中。
表1样品的抗菌活性
本发明采用液相等离子体技术成功地制备出了二硼化钪纳米粒子。与商用二硼化钪相比,二硼化钪纳米粒子具有更强的抗菌活性。抗菌活性的增强归因于其具有较大的比表面积。此外,二硼化钪纳米粒子对雷氏普罗威登斯菌的抗菌活性比丁胺卡那霉素和硫酸威替米星强。二硼化钪纳米粒子较强的雷氏普罗威登斯菌抑菌功能使其有望在烧伤、创伤和尿道感染等临床治疗领域方面得到广泛应用。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (4)
1.一种二硼化钪纳米粒子的制备方法,其特征在于:所述制备方法的具体步骤如下:
(1)将1.8mmol ScCl3加入24mL1-丁基-3-甲基咪唑硫氰酸盐离子液体中,在氩气保护下搅拌17分钟,以形成溶液;
(2)在氩气保护下把步骤(1)的混合液中转入50mL反应釜,通入硼烷,使硼烷与ScCl3的摩尔比为3.5-6.5:1,密闭反应釜;
(3)开启液相等离子体,功率为450-750W,对步骤(2)反应釜中的混合溶液在室温下进行处理25-55min后得到二硼化钪纳米粒子粗品;
(4)将产物用去离子水洗涤三次,再用无水乙醇洗涤三次,干燥备用。
2.如权利要求1所述的二硼化钪纳米粒子的制备方法,其特征在于:步骤(2)中,所通入硼烷与ScCl3的摩尔比为5:1。
3.如权利要求1所述的二硼化钪纳米粒子的制备方法,其特征在于:步骤(3)中,液相等离子体的功率为600W。
4.如权利要求1所述的二硼化钪纳米粒子的制备方法,其特征在于:步骤(3)中,反应时间为40min。
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