CN115154600A - 一种钆掺杂氧化钨纳米球的制备方法及应用 - Google Patents
一种钆掺杂氧化钨纳米球的制备方法及应用 Download PDFInfo
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Abstract
本发明涉及功能纳米材料技术领域,公开了一种钆掺杂氧化钨纳米球的制备方法和应用。其制备方法为溶剂热法,将氯化钨粉末加入到正丙醇溶液中并磁力至完全溶解,然后再加入六水硝酸钆粉末,搅拌至完全溶解后得到黄色透明溶液,将其转移至水热反应釜并放置在烘箱内反应,最后通过洗涤干燥处理得到非化学计量比W18O49‑Gd球形纳米材料。该方法合成工艺简单,无需表面活性剂(如聚乙二醇、聚乙烯吡咯烷酮、普朗尼克F127等)的修饰即可得到尺寸均匀的纳米球,所得到的纳米球平均尺寸在50 nm。材料在近红外光照射下表现出优异的光热性能,同时Gd离子的引入使以氧化钨为基体的纳米复合材料兼具MRI成像功能,有效解决纯氧化钨的单一CT成像对人体软组织分辨力较低的问题,在肿瘤的可视化光热治疗领域具有很大的应用前景。
Description
技术领域
本发明涉及功能纳米材料技术领域,公开了一种钆掺杂氧化钨纳米球的制备方法及应用。
背景技术
光热治疗是一种新型的癌症治疗方法,它是采用通过近红外波段的激光照射肿瘤部位,通过光热剂的光热效应,将激光的能量转化成热能,进而达到杀死肿瘤细胞的目的。
非化学计量比的氧化钨(WO3-x)纳米粒子由于其具有特殊的结构缺陷,粒子中同时存在W6+、W5+以及W4+三种价态的W元素,导致其既有优异的局部表面等离子共振(LSPRs)又在近红外光谱区域有很强的吸收能力,目前已经作为光催化剂、光热转换剂等应用于环境学、医学方面等方面。同时W因为原子序数较大可实现CT成像诊断功能,因此,W18O49本身作为光热剂的同时也可成为CT成像造影剂。钆(Gd)是一种常见的核磁共振(MRI)造影剂,可以明显改善病变的检测及定性,特别是检测肿瘤性病变。
目前医用造影剂只能满足于单一的CT成像或MRI成像。CT成像比MRI成像空间分辨率高,但是只能辨别有密度差别的组织,对软组织分辨能力不高。而MRI成像则对软组织有较好的分辨能力,如脂肪、肌肉、软骨、筋膜等,并且对软组织的成像能力高于CT数倍。但是在氢原子缺乏或者含量很少的组织,如致密的骨骼、钙化、含有气体的肺部等均无法成像。所以CT成像与MRI成像互相不能取代,二者相辅相成。因此,目前需要一种能够同时用于CT和MRI双模式成像的造影剂。
为解决上述问题,本发明采用一步溶剂热法制备了W18O49-Gd纳米材料,并探究其光热转化性能和体外成像功能,获得了一种在光热治疗的同时实现CT和MRI双模式成像的光热诊疗剂。
发明内容
本发明公开了一种钆掺杂氧化钨纳米球的制备方法及应用,探讨了W18O49-Gd的形貌、光热转换性能、磁性以及MRI成像性能。该材料形貌良好,尺寸均匀,表现出优异的光热性能和体外成像功能。
本发明通过以下技术方案实现:
一种钆掺杂氧化钨纳米球的制备方法,主要包括以下步骤:
(1)称取一定质量的氯化钨粉末放入烧杯中,然后向烧杯中加入正丙醇溶液,用保鲜膜封口后磁力搅拌至完全溶解;
(2)称取一定质量的六水硝酸钆粉末加入到步骤(1)所配置的混合溶液中,磁力搅拌至完全溶解,将完全溶解后的黄色透明溶液转移至聚四氟乙烯内衬的不锈钢反应釜并密封,将反应釜放入烘箱中保温一段时间,然后随炉却至室温;
(3)将步骤(2)得到的溶液取出离心后倒掉上清液,将沉淀洗涤,然后将洗干净的沉淀放置于真空干燥箱干燥,得到蓝色固体粉末。
其中优选,步骤(1)中所述氯化钨质量为0.2 g,正丙醇溶液体积为40 mL。
其中优选,步骤(1)中所述磁力搅拌时间为20-30 min。
其中优选,步骤(2)中所述六水硝酸钆质量为0.0115 g。
其中优选,步骤(2)中无需加入表面活性剂,如聚乙二醇、聚乙烯吡咯烷酮、普朗尼克F127等。
其中优选,步骤(2)中所述磁力搅拌时间为20-30 min。
其中优选,步骤(2)中所述烘箱温度为每分钟5 oC匀速升温到200 oC,保温时间为24 h。
其中优选,步骤(3)中所述离心转速为8000-10000 rpm/min,离心时间为8-10min。
其中优选,步骤(3)中所述洗涤条件为去离子水和无水乙醇交替洗涤,洗涤次数为2-3次,。
其中优选,步骤(3)中所述干燥温度为60 oC,干燥时间为8-10 h。
其中优选,步骤(3)中所述形成的W18O49-Gd纳米材料为直径50 nm的均匀球形。
本发明的有益效果:
(1)本发明以氯化钨和六水硝酸钆为原料,正丙醇为溶剂,通过简单的一步溶剂热法,无需添加表面活性剂(如聚乙二醇、聚乙烯吡咯烷酮、普朗尼克F127等)修饰即可制备出形状均匀的球形W18O49-Gd纳米材料,实验可重复性高。
(2)光热升温曲线表明合成的W18O49-Gd纳米材料具有良好的光热效果,808 nm激光照射下10 min内可升温至 41.5 oC。磁滞回线表明具有超顺磁性,饱和磁化强度为48emu/g。同时Gd离子的引入使以氧化钨为基体的纳米复合材料兼具MRI成像功能,有效解决纯氧化钨的单一CT成像对人体软组织分辨力较低的问题。
附图说明
图 1为显示W18O49-Gd物相的XRD图
图2为显示W18O49-Gd球状形貌的TEM图。
图3为W18O49-Gd的光热曲线。
图4为W18O49-Gd的3Dmax模拟光照和CAD选点图。
图5为W18O49-Gd的MATLAB模拟光热扩散图。
图6为W18O49-Gd的磁滞回线。
图7为不同浓度(0, 162.5, 325, 750, 1500, 3000 μg/mL)下W18O49-Gd的T1序列的核磁共振成像照片。
具体实施方式
实施例1 本发明涉及一种钆掺杂氧化钨球形纳米材料的制备方法,包括以下步骤:
(1) 称取0.2 g的氯化钨粉末放入烧杯中,然后向烧杯中加入40 mL的正丙醇溶液,用保鲜膜封口后磁力搅拌20-30 min至完全溶解;
(2)称取0.0115 g六水硝酸钆粉末并加入到步骤一所配置的混合溶液中,磁力搅拌20-30 min至完全溶解,将完全溶解后的溶液转移至聚四氟乙烯内衬的不锈钢反应釜并密封,将反应釜放入烘箱随炉升温至200 oC并保温24 h,待反应结束后随炉冷却至室温;
(3) 将步骤(2)得到的溶液以8000-10000 rpm/min离心8-10 min后倒掉上清液,将沉淀用去离子水和无水乙醇交替洗涤2-3次,然后将洗涤干净的沉淀放置于60 oC的真空干燥箱干燥8-10 h,得到蓝色固体粉末。
对以上实施例制备的样品进行以下检测和分析:
图1为W18O49-Gd纳米结构XRD图。曲线均与标准卡片PDF# 71-2450峰位基本一致,主峰尖锐。说明反应产物的仍然以W18O49为基体,结晶性良好未产生其他物质。
图2为W18O49-Gd的TEM图样,从图中可以看出材料呈现大小相对均匀的球形,平均直径为50 nm。
实施例2 光热性能测试
将样品配置成1 mg/mL的溶液,利用808 nm近红外光照射样品10 min,并用测温枪每隔1 min采集温度记录实验数据。测试功率为1.8 W,测试温度为23 oC,测温枪与测试点距离为5 cm。图3为W18O49-Gd在808 nm近红外光照射下的温度时间变化曲线,在W18O49-Gd结构用808 nm近红外光的照射10 min后,从升温曲线可以看出温度达到了41.5 oC。
实施例3 3Dmax模拟光照测试
图4为W18O49-Gd纳米结构的3Dmax模拟光照和CAD选点图。
实施例4 MATLAB模拟测试
图5为实施例1中制备的W18O49-Gd纳米结构的MATLAB模拟光热扩散图。
实施例5 磁性测试
采用南京南大仪器公司生产的HH-20型振动样品磁强计对W18O49-Gd纳米结构进行磁性测试。图6为W18O49-Gd纳米结构的磁滞回线。观察图像可以看出,图中磁滞回曲线未出现磁滞现象,即没有剩磁和矫顽力的产生,说明制备的W18O49-Gd纳米结构表现为超顺磁性,饱和磁化强度为48 emu/g。
实施例6 核磁共振成像测试
实验设备为医用西门子3.0T核磁共振成像仪,温度为18-22 oC。取不同浓度W18O49-Gd的水溶液(0, 162.5, 325, 750, 1500, 3000 μg/mL)于离心管中置入成像仪器中。图7为W18O49-Gd纳米结构不同浓度下T1序列的核磁共振成像照片。测试过程中放入纯W18O49作为对比组,由于其在核磁下不具备成像效果,故用3Dmax作图补充,作为空白对照无成像效果。从图片中可以清晰的看出,W18O49-Gd成像均匀清晰,随着样品用量浓度的增大,成像逐渐清晰。测试应用仪器为医用核磁测试仪器,所以W18O49-Gd纳米结构有作为可视化癌症治疗纳米材料的潜力。
综上,本发明所制备的W18O49-Gd球形纳米材料具有良好的光热效果,同时具有CT和MRI双模式成像功能,在肿瘤可视化光热治疗领域具有良好的应用前景。
Claims (9)
1.一种钆掺杂氧化钨纳米球的制备方法,其方法包括以下步骤:
(1)称取一定质量的氯化钨粉末放入烧杯中,然后在烧杯中加入一定量的正丙醇溶液,用保鲜膜封口后放置于磁力搅拌器搅拌至完全溶解;
(2)称取一定质量六水硝酸钆粉末加入到步骤(1)所配置的混合溶液中,磁力搅拌至完全溶解,无需加入表面活性剂(聚乙二醇、聚乙烯吡咯烷酮、普朗尼克F127等);将完全溶解后的黄色透明溶液转移至聚四氟乙烯内衬的反应釜中,然后将反应釜放入烘箱中保温,反应结束后随炉冷却至室温;
(3)将步骤(2)得到的溶液离心、洗涤、干燥后得到W18O49-Gd球形纳米材料。
2.根据权利要求1所述的一种钆掺杂氧化钨纳米球的制备方法,其特征在于步骤(1)中氯化钨质量为0.2 g,正丙醇溶液体积为40 mL,搅拌时间为20-30 min。
3.根据权利要求1所述的一种钆掺杂氧化钨纳米球的制备方法, 其特征在于步骤(2)中称取六水硝酸钆0.0115 g。
4.根据权利要求1所述的一种钆掺杂氧化钨纳米球的制备方法,其特征在于,步骤(2)所述的搅拌时间为20-30 min。
5.根据权利要求1所述的一种钆掺杂氧化钨纳米球的制备方法,其特征在于步骤(2)中烘箱以每分钟5 oC匀速升温到200 oC,保温时间为24 h。
6.根据权利要求1所述的一种钆掺杂氧化钨纳米球的制备方法,其特征在于步骤(3)中离心转速为8000-10000 rpm/min,所述离心时间为8-10 min。
7.根据权利要求1所述的一种钆掺杂氧化钨纳米球的制备方法,其特征在于步骤(3)中洗涤条件为用去离子水和无水乙醇交替洗涤,所述洗涤次数为2-3次。
8.根据权利要求1所述的一种钆掺杂氧化钨纳米球的制备方法,其特征在于步骤(3)中干燥条件为温度60 oC,干燥时间为8 -10 h。
9.根据权利要求1所述的一种钆掺杂氧化钨纳米球的制备方法,其特征在于步骤(3)中在没有表面活性剂修饰下形成的W18O49-Gd纳米材料为直径50 nm的均匀球形。
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