CN105542747B - 一种含有高级脂肪酸的量子点复合材料及其制备方法 - Google Patents
一种含有高级脂肪酸的量子点复合材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种含有高级脂肪酸的量子点复合材料及其制备方法。该量子点复合材料包括透光性基质、量子点和二氧化硅纳米微球，所述量子点自组装在所述二氧化硅纳米微球的表面，所述二氧化硅纳米微球包括壳层和内核，所述壳层为SiO2，所述内核为高级脂肪酸。本发明的量子点复合材料，本发明的量子点材料不但能够保持一般量子点发光效率高、光化学稳定性等优异性质，而且发光强度还具有特定的温度敏感值，可用于对特定的温度进行关联或监测。本发明的量子点复合材料还具有很好的重复使用性，量子点不会脱落问题。
Description
技术领域
本发明涉及一种量子点复合材料，更具体地说，涉及一种含有高级脂肪酸的量子点复合材料及其制备方法。
背景技术
当材料尺寸减少到纳米量级时，由于其纳米效应，材料将产生许多新颖而独特的优于传统材料的各种功能特性，在微电子、生物工程、化工、医学等领域具有广泛的应用价值。
近几年,以过渡金属为激活离子的纳米发光材料，由于其优异的光学特性，如吸收波长宽且连续，荧光发射峰可调谐，荧光寿命长等，在发光器件、荧光成像、太阳能电池、荧光检测和生物标记等领域表现出广阔的应用前景。然而当量子点用于发光器件或荧光检测时，在25-100℃范围内，量子点吸收峰波长和光致发光光谱波长发生的红移一般均小于10nm。再者，虽然发光强度与温度具有一定的线性关系，但随温度变化，其发光强度非常小，在低于热猝灭温度下，较小的温度变化不会引起发光强度大幅增强或减弱。因此，现有技术不能制备出温度敏感性非常高的量子点。
发明内容
为了克服现有技术中的不足之处，本发明提供了一种温度敏感性非常高的含有高级脂肪酸的量子点复合材料。
本发明提供的一种含有高级脂肪酸的量子点复合材料，其包括透光性基质、二氧化硅层和量子点层，所述二氧化硅层位于所述透光性基质上，所述量子点层位于所述二氧化硅层上，所述二氧化硅层由二氧化硅纳米微球自组装而形成，所述量子点层由量子点自组装而形成，所述二氧化硅纳米微球包括壳层和内核，所述壳层为SiO2，所述内核为高级脂肪酸。
所述量子点为巯基羧酸修饰的量子点；所述二氧化硅纳米微球的表面经过 三氨基硅烷和聚合氯化铝改性处理，其中，三氨基硅烷的化学式为H2N-CH2-CH2-NH-CH2-CH2-NH-(CH2)3-Si-(OCH3)3。
在所述量子点复合材料中，所述SiO2与所述高级脂肪酸的重量比例为(0.2～1.2)：1。
所述量子点可以采用本领域常规使用的量子点。所述量子点为CdTe、CdSe、InP、InAs、CdSe/CdS、CdSe/ZnS、CdSe/ZnSe、CdTe/ZnS、CdHgTe/ZnS、HgTe/HgCdS量子点中的一种或几种。量子点的粒径可以为1-100nm，优选为2-20nm，但不限制于此。
所述二氧化硅层厚度为50nm～600nm，优选为60nm～500nm，所述量子点层厚度为2～150nm，优选为5～100nm；所述二氧化硅纳米微球的平均粒径为50nm～600nm，优选为60nm～500nm。
高级脂肪酸为C9～C18的高级脂肪酸，优选为癸酸、月桂酸、肉豆蔻酸、棕榈酸、软脂酸、珠光酯酸、硬脂酸、油酸、亚油酸中的一种或多种。
本发明还提供的上述含有高级脂肪酸的量子点复合材料的制备方法，该方法包括如下步骤：
(1)将高级脂肪酸和表面活性剂加入到乙醇水溶液中，然后加热使高级脂肪酸熔融并搅拌均匀，制得含有高级脂肪酸的乳化液，然后在所述乳化液中加入正硅酸乙酯，加入碱溶液调节pH至9～12，然后进行水解反应，搅拌、静置、过滤、洗涤、干燥后，即得到二氧化硅包覆高级脂肪酸的二氧化硅纳米微球；
(2)将所述二氧化硅纳米微球加入水中，超声震荡30min，得到二氧化硅纳米微球的分散液，将透光性基质垂直插入用于制备二氧化硅纳米微球的分散液中进行垂直生长，取出干燥，制得覆盖于透光性基质表面的二氧化硅层；
(3)将覆盖有二氧化硅层的透光性基质垂直放置于量子点的水溶液中，取出干燥，便得到量子点复合材料。
在(1)步骤中，所述高级脂肪酸、表面活性剂和乙醇水溶液重量比例为10：(0.1～3.0)：(20～100)，所述乙醇水溶液中乙醇与水的重量比为(1～5):1； 所述高级脂肪酸与正硅酸乙酯酸类催化剂的重量比例为10：(5～40)。
所述表面活性剂为聚乙二醇、蔗糖酯、聚山梨酯、十八烷基苯磺酸、十二烷基硫酸钠、十四烷基硫酸钠、十六烷基硫酸钠中的一种或多种，优选为十二烷基硫酸钠和/或十四烷基硫酸钠。
在(2)步骤中，所述量子点的水溶液为巯基羧酸修饰的量子点的水溶液。所述浸泡的时间为5min～240min。
在将所述二氧化硅纳米微球加入到量子点的水溶液之前，用聚合氯化铝溶液和三氨基硅烷溶液改性处理二氧化硅纳米微球，具体步骤如下：将覆盖有二氧化硅层的透光性基质放置于聚合氯化铝的溶液中，然后取出干燥，然后再加入到三氨基硅烷溶液中，然后取出干燥。其中，聚合氯化铝溶液的浓度0.20wt％～0.01wt％。所述三氨基硅烷溶液为含有0.5wt％～2.0wt％三氨基硅烷的乙醇溶液。聚合氯化铝溶液和三氨基硅烷溶液的用量浸没二氧化硅化纳米微球即可，但不限制于此。二氧化硅纳米微球与聚合氯化铝溶液质量比例可以为1：(5～20)。二氧化硅纳米微球与三氨基硅烷溶液质量比例可以为1：(5～20)。
所述量子点的水溶液为巯基羧酸修饰的水溶性量子点，其制备方法如下：将碲粉和硼氢化钠与水混合，将惰性气氛环境和恒温条件进行反应，制得量子点前驱液；将氯化镉溶解在水中，然后依次加入巯基羧酸和氢氧化钠溶液，得到混合液，将整个混合液移至高压釜内衬里，通氮除氧，然后将所述量子点前驱液加入到所述混合液中，在高压釜进行水热反应，得到所述巯基羧酸修饰的水溶性量子点。所述碲粉、硼氢化钠、氯化镉与巯基羧酸的摩尔比例为1:(20～60):(15～45):(6～15)。巯基羧酸优选为巯基乙酸、2-巯基丙酸和3-巯基丙酸。
与现有技术相比，本发明的具有如下优点：
(1)本发明的量子点复合材料，本发明的量子点不但能够保持一般量子点发光效率高、光化学稳定性等优异性质，而且发光强度还具有特定的温度敏感值，可用于对特定的温度进行关联或监测。
Claims (13)
1.一种含有高级脂肪酸的量子点复合材料，其特征在于，其包括透光性基质、二氧化硅层和量子点层，所述二氧化硅层位于所述透光性基质上，所述量子点层位于所述二氧化硅层上，所述二氧化硅层由二氧化硅纳米微球自组装而形成，所述量子点层由量子点自组装而形成，所述二氧化硅纳米微球包括壳层和内核，所述壳层为SiO2，所述内核为高级脂肪酸。
2.按照权利要求1所述的量子点复合材料，其特征在于：所述二氧化硅层的表面经过三氨基硅烷和聚合氯化铝改性处理，所述三氨基硅烷的化学式为H2N-CH2-CH2-NH-CH2-CH2-NH-(CH2)3-Si-(OCH3)3。
3.按照权利要求1或2所述的量子点复合材料，其特征在于：在所述量子点复合材料中，所述SiO2与所述高级脂肪酸的重量比例为(0.2～1.2)：1。
4.按照权利要求1或2所述的量子点复合材料，其特征在于：所述二氧化硅层厚度为50nm～600nm，所述量子点层厚度为2～150nm；所述二氧化硅纳米微球的平均粒径为50nm～600nm。
5.按照权利要求4所述的量子点复合材料，其特征在于：所述二氧化硅层厚度为60nm～500nm，所述量子点层厚度为5～100nm；所述二氧化硅纳米微球的平均粒径为60nm～500nm。
6.按照权利要求1或2所述的量子点复合材料，其特征在于：所述量子点为CdTe、CdSe、InP、InAs、CdSe/CdS、CdSe/ZnS、CdSe/ZnSe、CdTe/ZnS、CdHgTe/ZnS、HgTe/HgCdS量子点中的一种或几种；所述高级脂肪酸为C9～C18的高级脂肪酸。
7.按照权利要求6所述的量子点复合材料，其特征在于：所述高级脂肪酸为癸酸、月桂酸、肉豆蔻酸、棕榈酸、软脂酸、珠光酯酸、硬脂酸、油酸、亚油酸中的一种或多种。
8.一种如权利要求1-7中任意一项所述的含有高级脂肪酸的量子点复合材料的制备方法，其特征在于，该方法包括如下步骤：
(1)将高级脂肪酸和表面活性剂加入到乙醇水溶液中，然后加热使高级脂肪酸熔融并搅拌均匀，制得含有高级脂肪酸的乳化液，然后在所述乳化液中加入正硅酸乙酯，加入碱溶液调节pH至9～12，然后进行水解反应，搅拌、静置、过滤、洗涤、干燥后，即得到二氧化硅包覆高级脂肪酸的二氧化硅纳米微球；
(2)将所述二氧化硅纳米微球加入水中，超声震荡30min，得到二氧化硅纳米微球的分散液，将透光性基质垂直插入用于制备二氧化硅纳米微球的分散液中进行垂直生长，取出干燥，制得覆盖于所述透光性基质表面的二氧化硅层；
(3)将覆盖有二氧化硅层的透光性基质垂直放置于量子点的水溶液中，取出干燥，便得到量子点复合材料。
9.按照权利要求8所述的方法，其特征在于：所述高级脂肪酸、表面活性剂和乙醇水溶液重量比例为10：(0.1～3.0)：(20～100)，所述乙醇水溶液中乙醇与水的重量比为(1～5):1；所述高级脂肪酸与正硅酸乙酯的重量比例为10：(5～40)，所述表面活性剂为聚乙二醇、蔗糖酯、聚山梨酯、十八烷基苯磺酸、十二烷基硫酸钠、十四烷基硫酸钠、十六烷基硫酸钠中的一种或多种。
10.按照权利要求9所述的方法，其特征在于：所述表面活性剂为十二烷基硫酸钠和/或十四烷基硫酸钠。
11.按照权利要求8或9所述的方法，其特征在于：所述量子点的水溶液为巯基羧酸修饰的量子点的水溶液。
12.按照权利要求8或9所述的方法，其特征在于：在将覆盖有二氧化硅层的透光性基质垂直放置于量子点的水溶液之前，用聚合氯化铝溶液和三氨基硅烷溶液改性处理二氧化硅层，具体步骤如下：将覆盖有二氧化硅层的透光性基质放置于聚合氯化铝的溶液中，然后取出干燥，然后再放置于三氨基硅烷溶液中，然后取出干燥。
13.按照权利要求12所述的方法，其特征在于：所述聚合氯化铝溶液的浓度0.20wt％～0.01wt％，所述三氨基硅烷溶液为含有0.5wt％～2.0wt％三氨基硅烷的乙醇溶液。
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