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CN103233208B - The method of using the ion beam sputtering apparatus nanostructure film microstructure Legal - Google Patents

The method of using the ion beam sputtering apparatus nanostructure film microstructure Legal Download PDF

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CN103233208B
CN103233208B CN 201310146298 CN201310146298A CN103233208B CN 103233208 B CN103233208 B CN 103233208B CN 201310146298 CN201310146298 CN 201310146298 CN 201310146298 A CN201310146298 A CN 201310146298A CN 103233208 B CN103233208 B CN 103233208B
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CN 201310146298
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CN103233208A (en )
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陶海华
张双喜
乔延琦
蒋为桥
陈险峰
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上海交通大学
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Abstract

本发明提供了一种利用离子束溅射法制备微纳米结构薄膜的装置和方法,该装置包括离子束溅射装置和准直过滤装置,准直过滤装置与离子束溅射装置的样品架连接,准直过滤装置包括:圆盘、若干过滤网和多个圆环,圆盘的下表面与样品架连接,各圆环依次重叠设置在圆盘上表面,过滤网设置在各圆环之间。 The present invention provides an apparatus and a method of using the nanostructure film microstructure Preparation of ion beam sputtering, ion beam sputtering, the device comprising a collimating means and the filter means, the filter means and collimating the ion beam sputtering apparatus is connected to the sample holder collimating filter apparatus comprising: a disk, a plurality of filters and a plurality of rings, discs connected to the lower surface of the sample holder, each of the rings are sequentially superimposed on the surface of the disk is provided, the filter is disposed between the ring . 本发明能够有效提高微纳米结构薄膜的质量,在纳米集成回路领域具有重要的应用价值。 The present invention can effectively improve the quality of the nanostructure film microstructure, it has important applications in the field of nano integrated circuit.

Description

利用离子束溅射法制备微纳米结构薄膜的方法 The method of using the ion beam sputtering apparatus nanostructure film microstructure Legal

技术领域 FIELD

[0001] 本发明涉及微纳米结构薄膜制备技术,具体地,涉及一种利用离子束溅射法制备微纳米结构薄膜的装置及方法。 [0001] The present invention relates to a micro preparation technique nanostructure film, in particular, relates to an apparatus and method using an ion beam sputtering apparatus legal nanostructure film microstructure.

背景技术 Background technique

[0002] 最近十几年,随着微纳米加工技术的迅速发展,其最小加工尺度向几十纳米迈进,并且加工精度也越来越高(可以达到几个纳米),这对微纳米结构的薄膜沉积技术提出了更高的要求。 [0002] the past ten years, with the rapid development of micro and nano processing technology, the minimum processing scale to tens of nanometers forward, and the machining accuracy is higher and higher (up to a few nanometers), which micro-nano structures thin film deposition techniques presented higher requirements. 比如,在新兴的纳米光子学、纳米电子学等前沿科学研究中,我们经常需要制备具有一定微纳米结构的金属薄膜。 For example, in the emerging nano photonics, nano-electronics and the like Frontier Scientific, we often desirable to prepare a metal thin film having a certain microstructure nanostructure. 在这一领域的基础研究中,蒸镀技术(如热蒸镀、电子束蒸镀)由于产生的原子、原子团簇等粒子的能量较低,其对光刻胶掩膜的损坏较小,易于脱膜,因而目前得到较为广泛的应用。 Based on the research in this field, vapor deposition techniques (e.g. thermal evaporation, electron beam deposition) due to the energy generated by atomic particles, clusters, etc. is low, less damage to the photoresist mask which is easy to stripping, which is currently been more widely used. 但是,采用这种技术沉积薄膜存在一定的问题,比如薄膜与基底的结合力相对较差以及原材料利用率低等问题,这将会在未来纳米集成回路的产业化过程中成为人们不可回避的问题。 However, there are some problems using this technique thin film is deposited, such as adhesion to the substrate film of relatively poor utilization of raw materials and low problem, it will become of unavoidable in the process of industrialization integrated circuit in the future nano .

[0003] 溅射镀膜是一种重要的薄膜沉积工艺,它与蒸镀一起构成物理气相沉积的两种重要技术,其在目前的工业化生产中发挥着举足轻重的作用。 [0003] sputtering a thin film deposition process is important, it is configured with the vapor deposition two important physical vapor deposition techniques, which plays an important role in the current industrial production. 大面积薄膜沉积工艺或微机电系统(Micro-Electro-Mechanical Systems,简称MEMS)中用到的图形结构一般在几个微米以上,物理气相溅射薄膜沉积技术由于节省原材料、薄膜与基底结合牢固以及致密性好等优点而在这一领域的科研和工业化生产中发挥着重要的作用。 Large area thin film deposition process or a microelectromechanical system (Micro-Electro-Mechanical Systems, MEMS) consist graph structure used in a few microns or more typically, a physical vapor deposition techniques, sputtering a thin film material saving since the film is firmly bonded to the substrate, and It plays an important role in the production of dense and good in the field of scientific research and industrialization. 物理溅射镀膜技术尽管具有上述蒸镀技术不可比拟的优点,但是在制备尺寸越来越小的纳米结构单元的基础研究中,这种技术却几乎不为人们所采用。 While physical sputtering technique has incomparable advantages of the vapor deposition techniques, but in the preparation of an increasingly smaller size of nano basic structural unit, but this technique is hardly used for people. 众所周知,相对于蒸镀过程而言,溅射镀膜过程中的原子、原子团簇等粒子能量大约是其几十倍。 It is well known with respect to the vapor deposition process, sputtering process atom clusters and other particle energy is about a few times thereof. 当制备的图形尺寸越来越小时,其光刻胶掩膜的厚度也相应变薄(具体来说,光刻胶掩膜的厚度不超过图形尺寸的三倍)。 As smaller and smaller feature sizes is prepared, its thickness is correspondingly thinner photoresist mask (specifically, the thickness of the photoresist mask pattern size is not more than three times). 因此,物理溅射镀膜过程中的高能量粒子将对这种相对很薄的光刻胶掩膜产生巨大破坏作用,特别是对微纳米结构的边缘部分,同时它也给脱膜工艺造成困难,从而导致微纳米结构薄膜的质量迅速降低。 Thus, high energy particle physics sputtering process that will produce a relatively thin photoresist mask could be devastating, especially on the edge portion of the micro-nano structures, and it also causes difficulties to the stripping process, resulting in reduced quality nanostructure film microstructure rapidly.

[0004] 如果能够降低溅射技术中高能量的粒子对光刻胶掩膜的破坏作用,就可以将这种溅射镀膜工艺用于微纳米结构薄膜的制备过程中。 [0004] If the sputtering technique can reduce the destructive effects of high-energy particles in the photoresist mask, which may be sputtering process for the preparation of nanostructured thin film microstructure. 具体而言,主要需要解决以下两个方面的问题:首先,降低溅射粒子在沉积薄膜时的能量;其次,进一步增强溅射粒子的方向性,减少斜入射粒子对光刻胶边缘产生的巨大破坏。 Specifically, the following two main problems need to be addressed: Firstly, when reducing the energy of sputtered particles deposited film; secondly, to further enhance the directivity of the sputtered particles, reducing the oblique incident particle generating photoresist edges enormous damage. 本发明中,以离子束溅射镀膜技术为例,通过在这套设备中增置一套准直过滤装置,可以明显提高微纳米结构薄膜的质量。 The present invention, the ion beam sputtering technique, for example, by increasing the linear filter means is set in this apparatus a registration, it can significantly improve the quality of the nanostructure film microstructure. 这种技术简便可行,不仅能够提高微纳米结构薄膜的质量,而且能够利用目前产业化的物理溅射设备进一步推动纳米集成回路的工业化进程。 This technique is simple and feasible, not only to improve the quality of micro and nano structure of the film, but also able to take advantage of the current industrialization of the physical sputtering equipment to further promote the industrialization of nanometer integrated circuits.

发明内容 SUMMARY

[0005] 针对现有技术中的缺陷,本发明的目的是提供一种利用离子束溅射法制备微纳米结构薄膜的装置及方法。 [0005] For the prior art drawbacks, the object of the present invention is an apparatus and method Sputtering microstructure provides a nanostructure film with an ion beam.

[0006] 根据本发明的一个方面,提供一种利用离子束溅射法制备微纳米结构薄膜的装置,包括离子束溅射装置和准直过滤装置,准直过滤装置与离子束溅射装置的样品架连接,准直过滤装置包括:圆盘、若干过滤网和多个圆环,圆盘的下表面与样品架连接,各圆环依次重叠设置在圆盘上表面,过滤网设置在各圆环之间。 [0006] In accordance with one aspect of the present invention, there is provided an apparatus for ion beam sputtering apparatus SPUTTERING SYSTEM microstructure using a nanostructure film, including ion beam sputtering apparatus and the collimating filter means, the filter means and the collimation of the ion beam the sample holder is connected, the collimating filter apparatus comprising: a disk, a plurality of filters and a plurality of rings, discs connected to the lower surface of the sample holder, each of the rings are sequentially superimposed on the surface of the disk is provided, the filter is provided in each circle between the rings.

[0007] 优选地,圆盘和圆环上均设置有开孔,圆盘和圆环通过开孔由螺钉固接至样品架。 [0007] Preferably, the disc and ring are provided has openings, fixed by a screw ring disc and connected to the sample holder through the opening.

[0008] 优选地,过滤网的数量为一个,圆环的数量为两个;或过滤网的数量为两个,圆环的数量为三个。 [0008] Preferably, the filter is a number, the number of rings is two; or the number of filters is two, the number of rings is three.

[0009] 优选地,圆盘的直径为4英寸,厚度为3mm。 [0009] Preferably, a disc diameter of 4 inches and a thickness of 3mm.

[0010] 优选地,过滤网为正方形,其中心网孔部分为圆形,且网孔为六角形结构。 [0010] Preferably, the filter is a square, the central mesh portion is circular and hexagonal mesh structure.

[0011] 优选地,过滤网的厚度为50 μΐΉ,边长为50mm,中心网孔部分直径为42mm,网孔孔径为100 μ m,肋宽为40〜50 μ m。 [0011] Preferably, the filter has a thickness of 50 μΐΉ, side length of 50mm, the central mesh portion having a diameter of 42mm, a mesh aperture of 100 μ m, rib width is 40~50 μ m.

[0012] 优选地,圆环外径为4英寸,内径为45mm,厚度为3mm。 [0012] Preferably, the ring outer diameter of 4 inches, an inner diameter of 45mm, thickness of 3mm.

[0013] 优选地,圆盘、过滤网和圆环均采用不锈钢材料制成。 [0013] Preferably, the disk, and an annular filter are made of stainless steel.

[0014] 根据本发明的另一个方面,提供一种利用离子束溅射法制备微纳米结构薄膜的方法,包括以下步骤: [0014] According to another aspect of the present invention, there is provided a method nanostructure film microstructure prepared utilizing ion beam sputtering, comprising the steps of:

[0015] 步骤1:制备具有光刻胶聚甲基丙烯酸甲酯掩膜的样品; [0015] Step 1: Samples having a polymethyl methacrylate resist mask prepared;

[0016] 步骤2:打开离子束溅射设备的主电源,充入氮气,打开真空腔室; [0016] Step 2: Turn on the main power supply of the ion beam sputtering apparatus, purged with nitrogen, opening the vacuum chamber;

[0017] 步骤3:将步骤1制备的样品固定于准直过滤装置的圆盘上,将过滤网夹持在圆环之间,并将准直过滤装置固定于离子束溅射装置的样品架; [0017] Step 3: A sample prepared in Step 1 is fixed to the disk collimating filter device, the filter is clamped between the ring and the collimator device is fixed to a sample holder filtered ion beam sputtering apparatus ;

[0018] 步骤4:依次开启真空腔室样品台的水冷系统和机械栗电源,当真空度高于IPa后,开启分子栗;当真空腔室本底真空度达到2*10 4Pa后,开启离子束溅射沉积设备; [0018] Step 4: Open water cooling system and turn the power Li mechanical vacuum chamber of the sample stage, when the degree of vacuum is higher than IPa, open molecular Li; true after the hollow chamber to reach a vacuum of 2 * 10 4Pa, open ion beam sputtering deposition apparatus;

[0019] 步骤5:溅射完成后,依次关闭分子栗和机械栗,充入氮气,取出样品,将样品置于丙酮试剂中浸泡约5个小时,去除PMMA电子束光刻胶,并依次用丙酮、乙醇以及去离子水清洗,最后用氮气吹干。 [0019] Step 5: After the completion of sputtering, and turn off the molecular machinery Li Li, flushed with nitrogen, the sample was removed, the sample was placed in reagent acetone soak for about 5 hours, PMMA electron beam resist is removed, and washed sequentially with acetone, ethanol, and rinsed with deionized water, and finally blown dry with nitrogen.

[0020] 优选地,步骤4中,离子束溅射的工艺参数为: [0020] Preferably, the step of ion beam sputtering process parameters to 4:

[0021] 离子能量:850eV ;离子束电流:70mA ;中和电流:91mA ; [0021] Ion energy: 850eV; Ion beam current: 70mA; and Current: 91mA;

[0022] 工作气体和压力:02;1.9*10 2Pa ; [0022] and the working gas pressure: 02; 1.9 * 10 2Pa;

[0023]沉积时间:Cr 为20sec, Ag 为80sec ; [0023] Deposition time: Cr is 20sec, Ag is 80sec;

[0024] 派射间隔:每派射60sec后间歇5min。 [0024] send the exit of intervals: every send intermittently emitted 60sec after 5min.

[0025] 与现有技术相比,本发明具有如下的有益效果:本发明通过设计准直过滤装置并设置在离子束溅射设备的样品架上,不仅可以有效阻止大角度斜入射粒子在基底上的沉积,降低其对光刻胶掩膜(特别是其边界部分)产生的破坏作用,而且能够阻止离子束轰击靶材后产生的大尺寸原子团簇等在基底上的沉积,从而有效提高制备的微纳米结构薄膜质量。 [0025] Compared with the prior art, the present invention has the following advantages: the present invention, by designing the collimating filter means and a sample holder disposed in an ion beam sputtering apparatus, not only can effectively prevent a large substrate particles incident angle of the swash deposited on, reducing the damaging effects on the photoresist mask (in particular its boundary portion) is generated, and can prevent the deposition of the generated ion beam bombard the target and other large clusters on the substrate, thereby effectively improving the preparation of film quality micro-nano structures. 本发明对于拓展以物理气相溅射技术为核心的镀膜工艺在微纳米结构元件以及未来微纳米集成回路中的应用具有重要意义。 The present invention is of great significance in the application of micro-nano structures, and the next element micro-nano integrated circuit for expanding sputtering physical vapor coating process technology as the core.

附图说明 BRIEF DESCRIPTION

[0026] 通过阅读参照以下附图对非限制性实施例所作的详细描述,本发明的其它特征、目的和优点将会变得更明显: [0026] By reading the following detailed description of non-limiting embodiments given with reference to the following figures, other features of the present invention, objects and advantages will become more apparent:

[0027]图1为本发明利用离子束溅射法制备微纳米结构薄膜的装置的结构示意图; [0027] FIG schematic structural diagram of an ion beam apparatus 1 Preparation microstructure nanostructure film by sputtering of the present invention;

[0028]图2为本发明实施例的准直过滤装置的结构分解图; Structure collimating filter device [0028] FIG. 2 is an exploded view of an embodiment of the invention;

[0029] 图3为本发明实施例的过滤网结构示意图; Filter structure [0029] FIG. 3 is a schematic view of an embodiment of the present invention;

[0030]图4为采用本发明中准直过滤装置前、后制备的微纳米结构图形的扫描电子显微镜(SEM)形貌图比较:(a)为不采用准直过滤装置;(b)为采用单层过滤网准直过滤装置; [0030] FIG 4 before the present invention employing collimating filter means, micro-nano pattern structure after preparation of a scanning electron microscope (SEM) comparison topography: (a) is not employed collimation filter means; (b) is a single-layer filter collimating filter means;

(c)为采用双层过滤网准直过滤装置; (C) a double filter employing collimating filter means;

[0031] 图5为利用本发明中采用双层过滤网准直过滤装置沉积的微纳米结构阵列的光学形貌图。 [0031] FIG. 5 is a view of the invention with the optical morphology of the double-layer filters quasi microstructure array of nanostructures deposited linear filtering means.

[0032] 图中:1为样品架,2为准直过滤装置,3为圆盘,4为过滤网,5为圆环。 [0032] FIG: 1 is a sample holder, a collimating filter device 2, a disk 3, 4 of the filter, 5 is a ring.

具体实施方式 detailed description

[0033] 下面结合具体实施例对本发明进行详细说明。 Specific embodiments of the present invention will be described in detail [0033] below in conjunction. 以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。 The following examples will assist those skilled in the art a further understanding of the invention, but do not limit the present invention in any way. 应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。 It should be noted that one of ordinary skill in the art, without departing from the spirit of the present invention, further modifications and changes may be made. 这些都属于本发明的保护范围。 All these fall within the scope of the present invention.

[0034] —种利用离子束溅射法制备微纳米结构薄膜的装置,包括离子束溅射装置和准直过滤装置2,准直过滤装置2与离子束溅射装置的样品架1连接,准直过滤装置2包括:圆盘3、两个过滤网4和三个圆环5,圆盘3的下表面与样品架1连接,各圆环5依次重叠设置在圆盘3的上表面,过滤网4设置在各圆环3之间。 [0034] - species using an ion beam sputtering apparatus Micromulsion legal nanostructure film, including ion beam sputtering apparatus and the collimating filter device 2, the collimating filter means 2 connected to the sample holder and the ion beam sputtering apparatus 1, the quasi- linear filter means 2 comprising: a disc 3, two filters 4 and three rings 5, the lower surface of the disc 3 and the sample rack 1 is connected to each of the ring 5 are sequentially superimposed on the surface of the disc 3 is provided, filtered 4 is provided between each network ring 3.

[0035] 圆盘3的下表面与样品架1连接,上表面用于放置和固定样品,圆盘3的直径为4英寸,厚度为3mm。 [0035] The lower surface of the disc 3 and the sample rack 1 is connected to the upper surface for placing and fixing the sample, the diameter of the disk 3 of 4 inches and a thickness of 3mm.

[0036] 如图3所示,其为过滤网的结构示意图。 [0036] As shown, the filter which is a schematic structural diagram of Fig. 过滤网4的尺寸略大于圆环5的内径尺寸,过滤网4的外形为边长50mm的正方形,中心为直径42mm的过滤网,厚度约为50 μπι,网孔为六角形结构,网孔孔径约为100 μm,肋宽约为40 μπι〜50 μπι。 Filter ring 4 is slightly larger than the inner diameter 5 of the filter 4 through the outer shape of a square side length of 50mm, 42mm diameter is too center of the screen, a thickness of about 50 μπι, hexagonal mesh structure, the mesh aperture about 100 μm, a width of the rib 40 μπι~50 μπι.

[0037] 圆环5不仅能够与圆盘3 —起固定于离子束溅射装置的样品架1上,并且各圆环5之间能够紧密夹持过滤网4。 [0037] The annular disc 5 is not only capable of 3 - to the ion beam from the fixed sample holder on a sputtering apparatus, and the filter 4 can be closely sandwiched between the ring 5. 圆环5的外径为4英寸,内径为45mm,厚度为3mm。 5 the outer diameter of the ring 4 inches, an inner diameter of 45mm, thickness of 3mm.

[0038] 进一步地,圆环5和圆盘3分别具有三个直径均为3.5mm的开孔,三个开孔在圆周上均匀分别,能用M3螺钉将圆环5和圆盘3固定于样品架1上。 [0038] Further, the annular disc 3 and 5 each have three openings diameters are 3.5mm, three openings are uniformly on the circumference, the ring 5 can M3 screws and fixed to the disc 3 1 on the sample rack.

[0039] 更为具体地,圆盘3、过滤网4和圆环5均采用不锈钢材料制成。 [0039] More specifically, the disc 3, the filter 4 and the ring 5 are made of stainless steel.

[0040] 本实例中,采用了双层过滤网准直过滤装置2,包括两个过滤网4和三个圆环5。 [0040] In the present example, a double-layered filter collimation filter means 2, comprises two filters 4 and 5 three rings. 但是,需要说明的是,本发明并不限定具体的过滤网4和圆环5的数量。 However, it should be noted that the present invention is not limited to the specific number of through the filter 4 and 5 rings. 在实际应用中,根据实际需要选择具体的准直过滤装置2的结构,可以为双层过滤网,还可以为单层过滤网甚至多层过滤网,相应地,过滤网4和圆环5的数量可以为一个过滤网4和两个圆环5,或均为多个。 In practical applications, according to actual needs to select a particular filter means collimating structure 2, may be a double filter, the filter may also be a single or even a multilayer filter, respectively, the filter 4 and the ring 5 a number of filters may be two rings 4 and 5, or a plurality of both. 因此,以上采用双层过滤网准直过滤装置2只是一个实施例,并不用于限定本发明。 Thus, the above filter using double-collimating filter means 2 is only an embodiment, not intended to limit the present invention.

[0041] 本发明还提供一种利用离子束溅射法制备微纳米结构薄膜的方法,包括以下步骤: [0041] The present invention further provides a method of using an ion beam sputtering apparatus legal nanostructure film microstructure, comprising the steps of:

[0042] 步骤1:制备具有光刻胶聚甲基丙稀酸甲酯(Poly(methyl methacrylate),简称PMMA)掩膜的样品。 [0042] Step 1: Preparation of a resist polymethylmethacrylate (Poly (methyl methacrylate), referred to as PMMA) sample mask.

[0043] 步骤2:打开离子束溅射设备的主电源,充入氮气,打开真空腔室。 [0043] Step 2: Turn on the main power supply of the ion beam sputtering apparatus, purged with nitrogen, opening the vacuum chamber.

[0044] 步骤3:将步骤1制备的样品固定于准直过滤装置的圆盘上,将过滤网夹持在圆环之间,并将准直过滤装置固定于离子束溅射装置的样品架。 [0044] Step 3: A sample prepared in Step 1 is fixed to the disk collimating filter device, the filter is clamped between the ring and the collimator device is fixed to a sample holder filtered ion beam sputtering apparatus .

[0045] 步骤4:依次开启真空腔室样品台的水冷系统和机械栗电源,当真空度高于IPa后,开启分子栗;当真空腔室本底真空度达到2*10 4Pa后,开启离子束溅射沉积设备。 [0045] Step 4: Open water cooling system and turn the power Li mechanical vacuum chamber of the sample stage, when the degree of vacuum is higher than IPa, open molecular Li; true after the hollow chamber to reach a vacuum of 2 * 10 4Pa, open ion beam sputter deposition apparatus.

[0046] 具体地,离子束溅射的工艺参数为: [0046] In particular, the ion beam sputtering process parameters is:

[0047] 离子能量:850eV ;离子束电流:70mA ;中和电流:91mA ; [0047] Ion energy: 850eV; Ion beam current: 70mA; and Current: 91mA;

[0048] 工作气体和压力:02;1.9*10 2Pa ; [0048] and the working gas pressure: 02; 1.9 * 10 2Pa;

[0049]沉积时间:Cr 为20sec, Ag 为80sec ; [0049] Deposition time: Cr is 20sec, Ag is 80sec;

[0050] 派射间隔:每派射60sec后间歇5min。 [0050] send the exit of intervals: every send intermittently emitted 60sec after 5min.

[0051] 在以上溅射参数下,当不采用准直过滤装置时,薄膜的沉积速率为4nm/SeC ;加入单层过滤网准直过滤装置后,薄膜的沉积速率为2.6nm/sec ;加入双层过滤网准直过滤装置后,薄膜的沉积速率为l.Snm/sec。 [0051] In the above sputtering parameters, collimation When no filter means, the deposition rate of 4nm / SeC; After addition of single collimating filter filtration apparatus, the deposition rate is 2.6nm / sec; added after the double filter collimation filter means, the deposition rate is l.Snm / sec. 因而,采用本发明的准直过滤装置,为沉积相同厚度的薄膜,需要预先计算离子束溅射所需时间。 Thus, collimation filter means to the present invention, in order to deposit the same film thickness, it is necessary calculation time required for an ion beam sputtering.

[0052] 步骤5:溅射完成后,依次关闭分子栗和机械栗,充入氮气,取出样品,将样品置于丙酮试剂中浸泡约5个小时,去除PMMA电子束光刻胶,并用依次用丙酮、乙醇以及去离子水清洗,最后用氮气吹干。 [0052] Step 5: After the completion of sputtering, and turn off the molecular machinery Li Li, flushed with nitrogen, the sample was removed, the sample was placed in reagent acetone soak for about 5 hours, PMMA electron beam resist is removed, and washed with successively with acetone, ethanol, and rinsed with deionized water, and finally blown dry with nitrogen.

[0053] 对于上述利用离子束溅射装置沉积微纳米结构薄膜的技术,下面以广为大家关注的石墨稀纳米电极制备过程中的标记图案为例,具体说明如何在Si02 ( 290nm厚度)/Si基底上沉积厚度约为40nm的微纳米结构Cr/Ag薄膜: [0053] For the above-described deposited by the ion beam sputtering apparatus nanostructure film microstructure, electrodes prepared graphene nano widely below to our attention during the marking pattern, for example, specify how Si02 (290nm thickness) / Si micro-nano structures on the substrate Cr deposition thickness of about 40nm / Ag film:

[0054] (1)在边长约为10mm的Si02/Si基底上依次旋涂PMMA495和950两种类型的电子束光刻胶,其厚度分别为290nm和230nm,光刻胶掩膜总厚度为520nm。 [0054] (1) at a side of about 10mm Si02 / Si substrate sequentially spin-coated on PMMA495 and 950 two types of electron beam resist having a thickness of 290nm and 230nm, respectively, the total thickness of the photoresist mask 520nm.

[0055] (2)利用Zeiss Ultra55扫描电子显微镜以及配套的电子束光阑和图形发生器在这种具有(1)所述的光刻胶掩膜的基底上曝光尺寸为500-1000nm的标记图案,其曝光剂量为600。 [0055] (2) use of a scanning electron microscope Zeiss Ultra55 and supporting the diaphragm and the electron beam pattern generator in which a resist mask having an upper (1) exposing the substrate to a size of a marking pattern 500-1000nm that an exposure dose of 600.

[0056] (3)在异丙醇(IPA)和4-甲基_2_戊酮(MIBK)的混合试剂配制的显影液及IPA定影液中依次显影40秒和定影60秒,然后用氮气吹干。 [0056] (3) are sequentially developed in isopropanol (IPA) and 4-methyl _2_ amyl ketone (MIBK) mixed reagent preparation of the developer and fixer IPA for 40 seconds and a fixing for 60 seconds with nitrogen and then dry. IPA和MIBK的体积比为3:1。 MIBK and IPA volume ratio of 3: 1. 显影、定影后,标记图案转移到PMMA光刻胶掩膜上。 Development, post-fixing, the marking pattern is transferred to PMMA resist mask.

[0057] (4)打开离子束溅射设备的主电源,充入氮气,打开真空腔室。 [0057] (4) on the main power of the ion beam sputtering apparatus, purged with nitrogen, opening the vacuum chamber. 该离子束溅射设备为北京埃德万斯离子束技术研究所生产的LDJ-2A-F100-100系列双离子束溅射沉积系统。 The ion beam sputtering apparatus for the production of Beijing Institute Ed Vance ion beam technology LDJ-2A-F100-100 series dual ion beam sputtering system.

[0058] (5)将上述(1)至(3)步骤中制备的具有光刻胶掩膜的样品固定于准直过滤装置的圆盘上,然后将单个过滤网夹持于近邻样品的两个圆环之间(即采用单过滤网准直过滤装置),或者将两个过滤网依次夹持于三个圆环之间(即采用双过滤网准直过滤装置),最后将这套准直过滤装置固定于离子束溅射装置的样品架上。 [0058] (5) The above (1) to (3) having a sample preparation step of a photoresist mask is fixed to the disk collimating filter device, the filter is then clamped in a single two neighbor samples between the circular ring (i.e., a single collimating filter filtering device), the two filters sequentially or sandwiched between the three rings (i.e., dual filter collimation filter means), and finally this registration linear filter means is fixed to the sample holder of an ion beam sputtering apparatus.

[0059] (6)依次开启真空腔室样品台的水冷系统和机械栗电源。 [0059] (6) water cooling system sequentially turned on and the power vacuum chamber machine Li sample stage. 当真空度高于IPa后,开启分子栗;当真空腔室本底真空度达到2*10 4Pa后,开启离子束溅射沉积设备。 When the degree of vacuum is higher than IPa, open molecular Li; true after the hollow chamber to reach a vacuum of 2 * 10 4Pa, ion beam sputter deposition apparatus is turned on.

[0060] 离子束溅射工艺中的主要参数如下: [0060] The ion beam sputtering process in the main parameters are as follows:

[0061] 离子能量:850eV ;离子束电流:70mA ;中和电流:91mA ; [0061] Ion energy: 850eV; Ion beam current: 70mA; and Current: 91mA;

[0062] 工作气体和压力:1.9*10 2Pa的02; [0062] and the working gas pressure: 1.9 * 10 2Pa 02;

[0063]沉积时间:Cr 为20sec, Ag 为80sec ; [0063] Deposition time: Cr is 20sec, Ag is 80sec;

[0064] 派射间隔:每派射60sec后间歇5min。 [0064] send the exit of intervals: every send intermittently emitted 60sec after 5min.

[0065] (7)计算溅射时间,当溅射过程完成后,依次关闭分子栗和机械栗,充入氮气,取出样品。 [0065] (7) calculating the sputtering time, when the sputtering process is completed, and turn off the molecular machinery Li Li, flushed with nitrogen, the sample was removed.

[0066] (8)将样品置于丙酮试剂中浸泡约5个小时,去除PMMA电子束光刻胶,并用依次用丙酮、乙醇以及去离子水清洗,最后用氮气吹干。 [0066] (8) The sample is placed in reagent acetone soak for about 5 hours, PMMA electron beam resist is removed, and washed with successively washed with acetone, ethanol and deionized water, and finally blown dry with nitrogen.

[0067] 利用SEM观察上述离子束溅射设备制备的金属薄膜形貌图,比较采用准直过滤装置前、后制备的微纳米结构图形的形貌变化,如图4所示。 [0067] The metal thin film was observed by SEM morphology prepared FIG ion beam sputtering apparatus described above was used to compare the filtration device before collimation, morphological changes of the micro-nano pattern structure after the preparation, as shown in FIG. 可以看到,本发明的准直过滤装置能够明显改善利用离子束溅射设备沉积的微纳米结构薄膜的质量。 It can be seen collimating filter device according to the present invention can significantly improve the microstructure by the mass of the nanostructure film deposited by ion beam sputtering apparatus. 利用离子束溅射设备和采用双层过滤网准直过滤装置制备的微纳米结构标记图案阵列的光学形貌如图5所示,可以达到应用要求。 And an ion beam sputtering apparatus shown using double filtering filter collimating optical Microminiatute marking pattern array of nanostructures prepared in apparatus shown in FIG 5, the application requirements can be achieved.

[0068] 本发明通过在离子束溅射设备的样品架上增置一套准直过滤装置,可以有效阻止斜入射粒子对掩膜(特别是边界部分)产生的破坏作用以及阻止离子束轰击靶材时产生的大尺寸原子团簇等在基底上的沉积,从而提高微纳米结构薄膜的质量,在纳米集成回路领域具有重要的应用价值。 [0068] In the present invention, a sample holder by ion beam sputtering apparatus home by a collimating filter means, can effectively prevent the damaging effects of the oblique incident particle mask (particularly the boundary portion) and preventing generation of ion beam bombardment of the target generated when a large size sheet and the like clusters on the substrate is deposited, thereby improving the quality of the nanostructure film microstructure, it has important applications in the field of nano integrated circuit.

[0069] 以上对本发明的具体实施例进行了描述。 [0069] The foregoing specific embodiments of the invention have been described. 需要理解的是,本发明并不局限于上述特定实施方式,本领域技术人员可以在权利要求的范围内做出各种变形或修改,这并不影响本发明的实质内容。 Is to be understood that the present invention is not limited to the particular embodiments, those skilled in the art can make various changes and modifications within the scope of the appended claims, this does not affect the substance of the present invention.

Claims (1)

  1. 1.一种利用离子束溅射法制备微纳米结构薄膜的方法,应用离子束溅射装置和准直过滤装置,所述准直过滤装置与所述离子束溅射装置的样品架连接,所述准直过滤装置包括:圆盘、若干过滤网和多个圆环,所述圆盘的下表面与所述样品架连接,所述各圆环依次重叠设置在所述圆盘上表面,所述过滤网设置在所述各圆环之间;其特征在于,包括以下步骤:步骤1:制备具有光刻胶聚甲基丙烯酸甲酯掩膜的样品; 步骤2:打开离子束溅射设备的主电源,充入氮气,打开真空腔室; 步骤3:将步骤1制备的样品固定于准直过滤装置的圆盘上,将过滤网夹持在圆环之间,并将准直过滤装置固定于离子束溅射装置的样品架; 步骤4:依次开启真空腔室样品台的水冷系统和机械栗电源,当真空度高于IPa后,开启分子栗;当真空腔室本底真空度达到2X10 4Pa后,开启离子束溅射 A microstructure prepared by sputtering the nanostructure film of the ion beam method, an ion beam sputtering apparatus and apply collimation filter means, said collimating means and the filtered sample holder in the ion beam sputtering apparatus is connected to the collimating said filtration device comprising: a disk, a plurality of filters and a plurality of rings, the lower surface of the disk with the sample holder connected to a respective annular disposed sequentially superimposed on the surface of the disk, the said filter disposed between said annular ring; characterized by comprising the following steps: step 1: the sample of polymethyl methacrylate resist mask having prepared; step 2: open an ion beam sputtering apparatus the main power supply, flushed with nitrogen, opening the vacuum chamber; step 3: a sample prepared in step 1 is fixed to the disk collimating filter device, the filter is clamped between the ring and the stationary collimating filter means a sample holder in the ion beam sputtering apparatus; step 4: open water cooling system and turn the power Li mechanical vacuum chamber of the sample stage, when the degree of vacuum is higher than IPa, open molecular Li; true hollow chamber to reach a vacuum of 2X10 after 4Pa, ion beam sputtering open 积设备,离子束溅射的工艺参数为: 离子能量:850eV ;离子束电流:70mA ;中和电流:91mA ; 工作气体和压力:02;1.9X10 2Pa ; 沉积时间:Cr为20sec, Ag为80sec ; 派射间隔:每派射60sec后间歇5min ; 步骤5:溅射完成后,依次关闭分子栗和机械栗,充入氮气,取出样品,将样品置于丙酮试剂中浸泡约5个小时,去除PMMA电子束光刻胶,并依次用丙酮、乙醇以及去离子水清洗,最后用氮气吹干。 Plot apparatus, an ion beam sputtering process parameters are as follows: ion energy: 850eV; Ion beam current: 70mA; and Current: 91mA; and a working gas pressure: 02; 1.9X10 2Pa; deposition time: of Cr is 20sec, Ag is 80sec ; send shot interval: 60sec after each shot sent intermittently 5min; step 5: after the completion of sputtering, and turn off the molecular machinery Li Li, flushed with nitrogen, the sample was removed, the sample was placed in reagent acetone soak for about 5 hours, removed electron beam resist PMMA and sequentially with acetone, ethanol, and rinsed with deionized water, and finally blown dry with nitrogen.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5330628A (en) * 1990-01-29 1994-07-19 Varian Associates, Inc. Collimated deposition apparatus and method
CN101307430A (en) * 2008-07-04 2008-11-19 郑州大学 Energy filtrated magnetron sputtering plating method and apparatus for applying the method
CN203295598U (en) * 2013-04-24 2013-11-20 上海交通大学 Device for preparing micro-nano structure thin film by utilizing ion beam sputtering method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5330628A (en) * 1990-01-29 1994-07-19 Varian Associates, Inc. Collimated deposition apparatus and method
CN101307430A (en) * 2008-07-04 2008-11-19 郑州大学 Energy filtrated magnetron sputtering plating method and apparatus for applying the method
CN203295598U (en) * 2013-04-24 2013-11-20 上海交通大学 Device for preparing micro-nano structure thin film by utilizing ion beam sputtering method

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