CN111646428B - 一种3d微/纳米结构的构筑方法 - Google Patents
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Abstract
本发明公开了一种3D微/纳米结构的构筑方法,包括以下步骤:(1)在基板上固定材料源,抽真空处理;(2)聚焦电子束的焦点在上述步骤(1)的材料源表面0‑100nm的距离处,形成包含有电子束焦点和表层原子的界面局域区;(3)控制电子束的焦点按照设计的3D微/纳米结构逐点移动,实现3D微/纳米结构的构筑。本发明的构筑方法,利用聚焦电子束焦点热辐射调控材料源表层原子,使表面原子动能增加,进而克服表面能的约束,自表面逃逸,同时界面局域区原子密度的不均衡及势能差使材料源的表层原子向低密度区扩散,从而实现在微/纳米尺度下三维结构的实时构筑,对纳米技术及3D打印的融合发展起到推动作用,具有较好的应用推广价值。
Description
技术领域
本发明涉及一种纳米结构的构筑方法,尤其涉及一种3D微/纳米结构的构筑方法。
背景技术
在微/纳米尺度下,材料的电子、光子及声子运动规律受到其微观结构的限制,这种微/纳米结构的限域效应使其具有许多新颖的物理和化学性质,在信息、材料、能源和环境等领域具有广阔的应用前景。因此,微/纳米结构材料的加工制备技术倍受人们的关注。
为了实现对材料尺寸、组成和结构的精确控制,人们开发了一系列的合成和制备方法。大体上可分为自下而上和自上而下两大类。自下向上的方法,如气-液-固化学气相沉积、固-液-固工艺和自组装方法等,可以利用材料的固有属性,如晶体的定向生长,亲水性和疏水性等制备从埃到数百纳米的纳米材料,这类方法成本低,制备方便快捷等,能够为纳米器件构筑提供最基本的材料,但是在对材料结构和尺寸的精确调控方面较为欠缺,而且要形成功能性微/纳米器件,还需要后期复杂的纳米加工组装工艺;自上向下的纳米结构构筑方法以光刻和电子束刻蚀方法为代表,不仅在器件制造、大规模集成和可寻址性等方面具有很大的优势,而且在纳米结构的加工精度方面也取得了巨大的成功。然而,光刻技术的不足之处也是很明显的,如结构加工过程步骤繁琐复杂、需要多步的图形传输过程和严格的实验条件,而且缺乏灵活性,不能实时修改设计方案等,这显然不适用于由多种纳米材料组成的多功能集成器件,纳米系统基本单元之间的电路连接和三维微/纳结构实时的、高精度的加工等。
3D打印技术作为一种快速成型技术,可以实现高纵横比三维结构实时构筑。然而,大部分3D打印技术,如立体光刻(SL),熔融沉积制造工艺(FDM),选域激光烧结(SLS)、选择性沉积叠片等,加工精度都在100微米以上,不适用于微/纳米器件的构筑;Lewis等人采用三维喷射打印方法制备了微米以上级别的银电极。然而,在纳米尺度下,表面能的影响越来越重要,这种喷射打印方法的加工精度受到表面能及仪器喷墨探头孔径大小的影响,也不适用于微纳米器件的构筑。3D激光直写技术,基于多光子聚合反应硬化成型过程,可以实现100/200纳米的加工精度,但是原材料主要限于有机感光单体有机材料,直接结果为三维有机聚合物微纳米结构。要想实现金属氧化物半导体器件,还需要复杂的结构反转复制过程。目前,寻求一种实况的,可以在纳米尺度下对材料成型过程进行精确控制的微制备技术,实现3D半导体微纳米结构的打印构筑,是材料科学与工程和纳米技术学科上的难点之一。
发明内容
为了克服现有技术的不足,本发明的目的在于提供一种3D微/纳米结构的构筑方法,实现了3D微/纳米结构的实况打印,对纳米加工技术及3D打印领域的发展具有重要的意义。
本发明的目的采用如下技术方案实现:
一种3D微/纳米结构的构筑方法,包括以下步骤:
(1)在基板上固定材料源,抽真空处理;
(2)聚焦电子束的焦点在上述步骤(1)的材料源表面近邻位置0-100nm距离处,形成包含有电子束焦点和表层原子的界面局域区;
(3)控制电子束的焦点按照设计的3D微/纳米结构逐点移动,实现3D微/纳米结构的构筑。
进一步地,上述步骤(1)中材料源的材质为金属单质、金属原子和其他非金属原子构成的化合物中的一种。
进一步地,所述材料源为块状固体、薄膜、棒材、纳米线组成的粉体、纳米颗粒组成的粉体、纳米带组成的粉体中的一种。
进一步地,上述步骤(1)的基板由导体或者半导体制成。
进一步地,上述步骤(1)中抽真空至真空度为10-3-10-5Pa。
进一步地,上述步骤(2)中加速电压为1-30kV,工作距离3-20mm,电子束束斑1-50nm。
进一步地,上述步骤(3)中结合位移平台和聚焦扫描控制程序,控制电子束的焦点按设计的3D微/纳米结构逐点移动。所述位移平台可以是光栅测量或激光测量定位位移平台。
相比现有技术,本发明的有益效果在于:本发明涉及一种3D微/纳米结构的构筑方法,利用聚焦电子束焦点热辐射调控材料源表层原子,使表面原子动能增加,进而克服表面能的约束,自表面逃逸,同时界面局域区原子密度的不均衡及势能差使材料源的表层原子向低密度区扩散,结合光栅定位位移平台及相应的聚焦扫描程序,从而实现在微/纳米尺度下三维结构的实时构筑,解决了材料加工及3D打印领域3D微/纳米结构的构筑难题,把3D打印技术的加工精度扩展到纳米尺度,对纳米技术及3D打印的融合发展起到推动作用,具有较好的应用推广价值。
附图说明
图1为本发明一种3D微/纳米结构的构筑方法的原理示意图;
图2为构筑过程中,材料源(A)、电子束焦点(B)及界面局域区(C)的位置示意图;
图3为实施例1中在ZnO材料表面构筑的字母“ED”图案;
图4为实施例2中在氧化钴镍纳米线上构筑的植物种子胚芽状结构图;
图5为实施例3中在铜丝顶端构筑的纳米棒的结构图。
图中:1、电子束;11、电子束焦点;2、基板;3、材料源;4、纳米结构。
具体实施方式
下面,结合附图以及具体实施方式,对本发明做进一步描述,需要说明的是,在不相冲突的前提下,以下描述的各实施例之间或各技术特征之间可以任意组合形成新的实施例。
实施例1
一种3D微/纳米结构的构筑方法,包括以下步骤:
(1)取长宽均为1cm的硅片依次用超纯水、乙醇、丙酮各超声10分钟后作为基板2,在硅基板上采用磁控溅射镀膜的方法沉积一层厚度100nm的ZnO薄膜,以此ZnO薄膜作为构筑立体结构的材料源3,把沉积ZnO薄膜的硅基板放入电镜真空室抽真空,使真空度达到10- 4Pa;
(2)打开灯丝,调整电子束1状态及光栅位移平台,工作距离7mm,加速电压10kV,电子束束斑10nm,电子束1以70°角斜入射到ZnO表面(如图1所示),使电子束焦点11位于ZnO表面上方的近邻位置,和ZnO表面的距离为10nm(图2中的B区),电子束焦点11和ZnO表层原子形成界面局域区(图2中的C区),聚焦电子束焦点的热辐射活化界面局域区内的表层原子,表面原子动能增加,同时,在界面局域区内原子密度的不均衡及势能差使ZnO表面的活化原子向焦点扩散;
(3)通过光栅测量定位位移平台及聚焦扫描程序,控制聚焦电子束焦点按设计的字母结构逐点移动,形成相应的ZnO 3D字母结构,如图3所示为ZnO原子形成的纳米结构4“ED”字符。
实施例2
一种3D微/纳米结构的构筑方法,包括以下步骤:
(1)采用水热法合成氢氧钴镍多晶纳米线,然后在马弗炉中400摄氏度退火2小时,形成氧化钴镍多晶纳米线粉体,把氧化钴镍多晶纳米线分散到硅片基板上,作为生长纳米胚芽的源材料,把上述硅片基板放入电镜真空室抽真空,使真空度达到10-3Pa;
(2)打开灯丝,调整电子束状态及光栅位移平台,工作距离12mm,加速电压15kV,电子束束斑20nm,聚焦电子束,使电子束焦点位于氧化钴镍多晶纳米线粉体生长点的近邻位置,和氧化钴镍多晶纳米线粉体表面的距离为0nm,使电子束焦点和纳米线表面相切,电子束焦点和氧化钴镍多晶纳米线上的生长点表层形成界面局域区,聚焦电子束焦点的热辐射活化界面局域区内氧化钴镍的表层原子,表面原子动能增加,同时,在界面局域区内原子密度的不均衡使表面的活化原子向焦点扩散;
(3)通过光栅测量定位位移平台及聚焦扫描程序,控制电子束焦点按设计的植物种子胚芽结构逐点移动,形成相应的植物种子胚芽形状,如图4所示,图中a、b、c表示胚芽纳米结构的形成过程,c中可以看到完整的纳米胚芽结构。
实施例3
一种3D微/纳米结构的构筑方法,包括以下步骤:
(1)以铜质样品台作为基板,取一段铜丝,用力拉断,用导电胶带固定到铜质样品台上,以铜丝的断裂端作为纳米棒的生长点,把上述铜质样品台放入电镜真空室抽真空,使真空度达到10-5Pa;
(2)打开灯丝,调整电子束状态及光栅位移平台,工作距离20mm,加速电压30kV,电子束束斑50nm,聚焦电子束,使电子束焦点位于铜丝生长点的近邻位置,和铜丝生长点的距离为50nm,电子束焦点和铜丝生长点附近表层形成界面局域区,聚焦电子束焦点的热辐射活化界面局域区内的表层铜原子,表面铜原子动能增加,同时,在界面局域区内原子密度的不均衡使表面的活化铜原子向焦点扩散;
(3)通过激光测量定位位移平台及聚焦扫描程序,控制电子束焦点按设计的纳米棒形状逐点移动,形成相应的铜纳米棒,如图5所示,纳米棒直径约为25nm。
上述实施方式仅为本发明的优选实施方式,不能以此来限定本发明保护的范围,本领域的技术人员在本发明的基础上所做的任何非实质性的变化及替换均属于本发明所要求保护的范围。
Claims (6)
1.一种3D微/纳米结构的构筑方法,其特征在于,包括以下步骤:
(1)在基板上固定材料源,抽真空处理;
(2)聚焦电子束的焦点在上述步骤(1)的材料源表面0-100nm的距离处,加速电压为1-30kV,工作距离3-20mm,电子束束斑1-50nm,形成包含有电子束焦点和表层原子的界面局域区;
(3)控制电子束的焦点按照设计的3D微/纳米结构逐点移动,实现3D微/纳米结构的构筑。
2.根据权利要求1所述一种3D微/纳米结构的构筑方法,其特征在于,上述步骤(1)中材料源的材质为金属单质、金属原子和其他非金属原子构成的化合物中的一种。
3.根据权利要求2所述一种3D微/纳米结构的构筑方法,其特征在于,所述材料源为块状固体、薄膜、棒材、纳米线组成的粉体、纳米颗粒组成的粉体、纳米带组成的粉体中的一种。
4.根据权利要求1所述一种3D微/纳米结构的构筑方法,其特征在于,上述步骤(1)的基板为导体或者半导体材质。
5.根据权利要求1所述一种3D微/纳米结构的构筑方法,其特征在于,上述步骤(1)中抽真空至10-3-10-5Pa。
6.根据权利要求1所述一种3D微/纳米结构的构筑方法,其特征在于,上述步骤(3)中结合位移平台和聚焦扫描控制程序,控制电子束的焦点按设计的3D微/纳米结构逐点移动。
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