CN113981371A - 高SERS强度的Ag/SiO2共溅射单层膜制备方法 - Google Patents
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Abstract
本发明公开了高SERS强度的Ag/SiO2共溅射单层膜制备方法，包括以下步骤：(1)硅片亲水处理；(2)制备Ag/SiO2共溅射单层膜；(3)利用氢氟酸对Ag/SiO2共溅射单层膜进行腐蚀，得高SERS强度Ag/SiO2共溅射单层膜。本发明设计并制备得到了一种可实现比单层金属膜SERS增强效果更高的金属‑绝缘体共溅射膜(Ag/SiO2)，采用较为简单的磁控溅射，从而利用氢氟酸对二氧化硅的腐蚀性，使Ag/SiO2共溅射薄膜中的二氧化硅被不同程度腐蚀，从而留下不同颗粒大小和间隔的银纳米颗粒，提高其单层膜的SERS强度。
Description
技术领域
本发明涉及纳米材料制备技术领域，尤其是涉及高SERS强度的Ag/SiO2共溅射单层膜制备方法。
背景技术
利用磁控溅射、化学反应等技术可以实现不同程度上改善单层金属膜SERS强度较低的缺陷，制备简单可控，成本较低，可搭载在其他结构上，转移性较好。
磁控溅射是物理气相沉积(Physical Vapor Deposition，PVD)的一种。一般的溅射法可被用于制备金属、半导体、绝缘体等多材料，且具有设备简单、易于控制、镀膜面积大和附着力强等优点。它的工作原理是指电子在电场E的作用下，在飞向基片过程中与氩原子发生碰撞，使其电离产生出Ar正离子和新的电子；新电子飞向基片，Ar离子在电场作用下加速飞向阴极靶，并以高能量轰击靶表面，使靶材发生溅射。
表面增强拉曼散射(SERS)技术克服了传统拉曼光谱与生俱来的信号微弱的缺点，可以使得拉曼强度增大几个数量级。其增强因子可以高达1014～1015倍，足以探测到单个分子的拉曼信号，这些都是传统拉曼的灵敏度和测量速度不足以完成的。
目前最常用的金属是金和银，但是单层金属膜的SERS强度有限，其测试范围和大小都有很大的局限性。因此，在改进单层金属膜的SERS强度就有很大的意义，在环境监测、食品安全、临床检验及疾病诊断等众多领域中能有充分应用。
发明内容
本发明是为了解决现有技术的单层金属膜的SERS强度有限，其测试范围和大小都有很大的局限性的问题，提供了一种工艺步骤简单，可操作性强，能使SERS强度增强的高SERS 强度的Ag/SiO2共溅射单层膜制备方法。
为了实现上述目的，本发明采用以下技术方案：高SERS强度的Ag/SiO2共溅射单层膜制备方法，包括以下步骤：
(1)硅片亲水处理：将清洗后的硅片置于烧杯中，加入氨水、过氧化氢和去离子水的混合溶液中，煮至沸腾后保持煮沸，冷却后，倒出混合溶液，硅片用去离子水、无水乙醇反复超声。
(2)制备Ag/SiO2共溅射单层膜：将银靶和二氧化硅靶分别倾斜40°，同时向硅片溅射，在硅片表面生成Ag/SiO2共溅射单层膜。
(3)利用氢氟酸对Ag/SiO2共溅射单层膜进行腐蚀，得高SERS强度Ag/SiO2共溅射单层膜。
作为优选，步骤(1)中，所述清洗后的硅片通过以下步骤制得：用去离子水和无水乙醇分别浸泡干净硅片，超声处理。通过控制氢氟酸腐蚀时间能使二氧化硅产生不同程度的腐蚀，从而留下不同颗粒大小和间隔的银纳米颗粒，控制单层膜的SERS强度。
作为优选，步骤(1)中，混合溶液中，氨水、过氧化氢和去离子水的体积比为1:2:6。
作为优选，步骤(1)中，保持煮沸10～15分钟。
作为优选，超声时间为10～15min。
作为优选，步骤(2)中，开始前背景气压为4.5×10-4Pa，通入25sccm的Ar，溅射时背景气压为1.5Pa，银溅射功率10W，二氧化硅溅射功率为40W，溅射时间为10～120s。10～60s共溅射形成的是颗粒膜，70～120s形成的是连续膜；不同溅射功率下的银纳米颗粒大小不同，通过多次试验发现，银溅射功率10W能得到大小最合适的银颗粒。
因此，本发明具有如下有益效果：本发明设计并制备得到了一种可实现比单层金属膜 SERS增强效果更高的金属-绝缘体共溅射膜(Ag/SiO2)，采用较为简单的磁控溅射，从而利用氢氟酸对二氧化硅的腐蚀性，使Ag/SiO2共溅射薄膜中的二氧化硅被不同程度腐蚀，从而留下不同颗粒大小和间隔的银纳米颗粒，提高其单层膜的SERS强度。
附图说明
图1是实施例1中Ag/SiO2共溅射单层膜SEM图。
图2是实施例1中高SERS强度Ag/SiO2共溅射单层膜SEM图。
图3是实施例1中Ag/SiO2共溅射单层膜与高SERS强度Ag/SiO2共溅射单层膜的拉曼对比图。
图4是实施例2中Ag/SiO2共溅射单层膜SEM图。
图5是实施例2中高SERS强度Ag/SiO2共溅射单层膜SEM图。
图6是实施例2中Ag/SiO2共溅射单层膜与高SERS强度Ag/SiO2共溅射单层膜的拉曼对比图。
图7是实施例3中Ag/SiO2共溅射单层膜SEM图。
图8是实施例3中高SERS强度Ag/SiO2共溅射单层膜。
图9是实施例3中Ag/SiO2共溅射单层膜与高SERS强度Ag/SiO2共溅射单层膜的拉曼对比图。
具体实施方式
下面结合附图和具体实施方式对本发明做进一步的描述。
实施例1
(1)硅片亲水处理：将清洗后的硅片置于烧杯中，加入氨水、过氧化氢和去离子水的混合溶液中，混合溶液中，氨水、过氧化氢和去离子水的体积比为1:2:6，煮至沸腾后保持煮沸 10～15min，冷却后，倒出混合溶液，硅片用去离子水、无水乙醇反复超声10min；其中清洗后的硅片通过以下步骤制得：用去离子水和无水乙醇分别浸泡干净硅片，超声处理。
(2)制备Ag/SiO2共溅射单层膜：将银靶和二氧化硅靶分别倾斜40°，同时向硅片溅射，在硅片表面生成Ag/SiO2共溅射单层膜；开始前背景气压为4.5×10-4Pa，通入25sccm 的Ar，溅射时背景气压为1.5Pa，银溅射功率10W，二氧化硅溅射功率为40W，溅射时间为 50s，生成的Ag/SiO2共溅射单层膜SEM图如图1所示。
(3)利用质量百分数20％的氢氟酸对Ag/SiO2共溅射单层膜进行腐蚀，腐蚀时间为10s，得高SERS强度Ag/SiO2共溅射单层膜，高SERS强度Ag/SiO2共溅射单层膜的SEM图如图2所示。
Ag/SiO2共溅射单层膜与高SERS强度Ag/SiO2共溅射单层膜的拉曼对比图如图3所示。
实施例2
(1)硅片亲水处理：将清洗后的硅片置于烧杯中，加入氨水、过氧化氢和去离子水的混合溶液中，混合溶液中，氨水、过氧化氢和去离子水的体积比为1:2:6，煮至沸腾后保持煮沸 10～15min，冷却后，倒出混合溶液，硅片用去离子水、无水乙醇反复超声12min；其中清洗后的硅片通过以下步骤制得：用去离子水和无水乙醇分别浸泡干净硅片，超声处理。
(2)制备Ag/SiO2共溅射单层膜：将银靶和二氧化硅靶分别倾斜40°，同时向硅片溅射，在硅片表面生成Ag/SiO2共溅射单层膜；开始前背景气压为4.5×10-4Pa，通入25sccm 的Ar，溅射时背景气压为1.5Pa，银溅射功率10W，二氧化硅溅射功率为40W，溅射时间为 60s；生成的Ag/SiO2共溅射单层膜SEM图如图4所示。
(3)利用质量百分数20％的氢氟酸对Ag/SiO2共溅射单层膜进行腐蚀，腐蚀时间为10s，得高SERS强度Ag/SiO2共溅射单层膜，高SERS强度Ag/SiO2共溅射单层膜的SEM图如图5所示。
Ag/SiO2共溅射单层膜与高SERS强度Ag/SiO2共溅射单层膜的拉曼对比图如图6所示。
实施例3
(1)硅片亲水处理：将清洗后的硅片置于烧杯中，加入氨水、过氧化氢和去离子水的混合溶液中，混合溶液中，氨水、过氧化氢和去离子水的体积比为1:2:6，煮至沸腾后保持煮沸 10～15min，冷却后，倒出混合溶液，硅片用去离子水、无水乙醇反复超声15min；其中清洗后的硅片通过以下步骤制得：用去离子水和无水乙醇分别浸泡干净硅片，超声处理。
(2)制备Ag/SiO2共溅射单层膜：将银靶和二氧化硅靶分别倾斜40°，同时向硅片溅射，在硅片表面生成Ag/SiO2共溅射单层膜；开始前背景气压为4.5×10-4Pa，通入25sccm 的Ar，溅射时背景气压为1.5Pa，银溅射功率10W，二氧化硅溅射功率为40W，溅射时间为 70s；生成的Ag/SiO2共溅射单层膜SEM图如图7所示。
(3)利用质量百分数20％的氢氟酸对Ag/SiO2共溅射单层膜进行腐蚀，腐蚀时间为10s，得高SERS强度Ag/SiO2共溅射单层膜，高SERS强度Ag/SiO2共溅射单层膜的SEM图如图8所示。
Ag/SiO2共溅射单层膜与高SERS强度Ag/SiO2共溅射单层膜的拉曼对比图如图9所示。
以上所述的实施例只是本发明的一种较佳的方案，并非对本发明作任何形式上的限制，在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。
Claims (6)
1.高SERS强度的Ag/SiO2共溅射单层膜制备方法，其特征在于，包括以下步骤：
(1)硅片亲水处理：将清洗后的硅片置于烧杯中，加入氨水、过氧化氢和去离子水的混合溶液中，煮至沸腾后保持煮沸，冷却后，倒出混合溶液，硅片用去离子水、无水乙醇反复超声；
(2)制备Ag/SiO2共溅射单层膜：将银靶和二氧化硅靶分别倾斜40°，同时向硅片溅射，在硅片表面生成Ag/SiO2共溅射单层膜；
(3)利用氢氟酸对Ag/SiO2共溅射单层膜进行腐蚀，得高SERS强度Ag/SiO2共溅射单层膜。
2.根据权利要求1所述的高SERS强度的Ag/SiO2共溅射单层膜制备方法，其特征在于，步骤(1)中，所述清洗后的硅片通过以下步骤制得：用去离子水和无水乙醇分别浸泡干净硅片，超声处理。
3.根据权利要求1所述的高SERS强度的Ag/SiO2共溅射单层膜制备方法，其特征在于，步骤(1)中，混合溶液中，氨水、过氧化氢和去离子水的体积比为1:2:6。
4.根据权利要求1所述的高SERS强度的Ag/SiO2共溅射单层膜制备方法，其特征在于，步骤(1)中，保持煮沸10～15分钟。
5.根据权利要求1所述的高SERS强度的Ag/SiO2共溅射单层膜制备方法，其特征在于，超声时间为10～15min。
6.根据权利要求1所述的高SERS强度的Ag/SiO2共溅射单层膜制备方法，其特征在于，步骤(2)中，开始前背景气压为4.5×10-4Pa，通入25sccm的Ar，溅射时背景气压为1.5Pa，银溅射功率10W，二氧化硅溅射功率为40W，溅射时间为10～120s。
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