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Número de publicaciónCN103233208 B
Tipo de publicaciónConcesión
Número de solicitudCN 201310146298
Fecha de publicación13 Abr 2016
Fecha de presentación24 Abr 2013
Fecha de prioridad24 Abr 2013
También publicado comoCN103233208A
Número de publicación201310146298.2, CN 103233208 B, CN 103233208B, CN 201310146298, CN-B-103233208, CN103233208 B, CN103233208B, CN201310146298, CN201310146298.2
Inventores陶海华, 张双喜, 乔延琦, 蒋为桥, 陈险峰
Solicitante上海交通大学
Exportar citaBiBTeX, EndNote, RefMan
Enlaces externos:  SIPO, Espacenet
利用离子束溅射法制备微纳米结构薄膜的方法 Using the method of ion beam sputtering thin films prepared by micro nanostructure traducido del chino
CN 103233208 B
Resumen  traducido del chino
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 method using an ion beam sputtering Preparation of micro and nano structure of the film, the apparatus comprising an ion beam sputtering apparatus and collimating filters, filter device and collimated ion beam sputtering apparatus connected to the sample holder collimating filter device comprising: a disk, several filters and a plurality of rings, the lower surface of the sample holder disk connection, each ring in turn is superposed on the surface of the disk, 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 micro and nano structure of the film, it has important applications in the field of nanometer integrated circuits.
Reclamaciones(1)  traducido del chino
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,开启离子束溅射沉积设备,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。 An ion beam sputtered thin films prepared by microfabrication methods, application of ion beam sputtering apparatus and collimating filter means, said collimator means and filtering the sample holder of the ion beam sputtering device is connected, the filtering said collimating means comprising: a disk, a plurality of rings and a plurality of filters, the lower surface of the disc and connected to the sample holder, each of said rings in turn is superposed on the surface of the disc, the said filter disposed between said rings; characterized by comprising the following steps: step 1: Preparation of a sample having a polymethyl methacrylate resist mask; step 2: open the ion beam sputtering apparatus the main power supply, purged with nitrogen, open the vacuum chamber; step 3: a sample prepared in step 1 is fixed to the disc collimating filter device, the filter is clamped between the ring and the collimating filter unit to ion beam sputtering apparatus of the sample holder; step 4: open the vacuum chamber successively sample stage cooling system and mechanical power chestnut, when the degree of vacuum higher than IPa, open molecular chestnut; really hollow chamber background vacuum of 2X10 after 4Pa open ion beam sputtering deposition apparatus, an ion beam sputtering process parameters are as follows: ion energy: 850eV; ion beam current: 70mA; and current: 91mA; working gas and pressure: 02; 1.9X10 2Pa; deposition time : Cr is 20sec, Ag is 80sec; faction shot interval: 60sec after each shot sent intermittent 5min; step 5: after the completion of sputtering, and then click Close and molecular machinery chestnut chestnut, filled with nitrogen, the sample was removed, the sample is placed in acetone reagent soak for about 5 hours, to remove an electron beam resist PMMA and washed with acetone, ethanol, and deionized water, and finally blown dry with nitrogen.
Descripción  traducido del chino
利用离子束溅射法制备微纳米结构薄膜的方法 Using the method of ion beam sputtering thin films prepared by micro nanostructure

技术领域 TECHNICAL 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-nano structured thin film preparation technology, in particular, it relates to an apparatus and method for ion beam sputtering film prepared micro and nano structure of a use.

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 last ten years, with the rapid development of micro-nano processing technology, the minimum processing dimension to move tens of nanometers, and more and more high precision (up to a few nanometers), which micro-nano structures thin film deposition techniques put forward 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 nanophotonics, nanoelectronics and other cutting-edge research, we often need to prepare the metal film has a micro and nano structures. 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。 On the basis of research in this area, the vapor deposition techniques (such as thermal evaporation, e-beam evaporation) due to the energy generated by atomic, atomic particles such as clusters of low, its small damage to the photoresist mask, easy 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 deposition film, such as film and substrate adhesion and relatively poor and low utilization of raw materials, which will become an unavoidable issue in the process of industrialization in the future nanometer integrated circuits .

[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] is an important sputtering film deposition process, which constitutes a physical vapor deposition and deposition of two important technologies together, which plays a pivotal 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 MEMS (Micro-Electro-Mechanical Systems, referred to as MEMS) structure used in graphics are typically in the micron, physical vapor deposition sputtered film due to the material saving, and film and substrate firmly combined dense and good in the field of scientific research and industrial production plays an important role. 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。 Physical sputtering technique despite having the deposition technology incomparable advantages, but in the manufacture of ever-smaller nanostructures basic research units, this technology is hardly used by 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。 As we all know, with respect to the deposition process, the sputtering process of atom, atomic particles such as energy clusters around its few times. 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 prepared, its thickness is correspondingly thinned resist 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。 Therefore, the physical sputtering process will be high-energy particles such relatively thin photoresist mask enormous destructive effect, especially on the edge portion of micro and nano structure, but it also caused difficulties for stripping process, resulting in micro and nano structure of the film quality decreased 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 damaging effects of high energy particles in the photoresist mask, it can be such a sputtering process for the preparation of micro-nano-structure thin film. 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 main need to address the following two aspects: First, reduce energy sputtered particles at the time of the deposited film; secondly, to further enhance the directionality of the sputtered particles, reducing the oblique incident particle to resist the enormous edge 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 set in a quasi-linear filter means in the equipment, can significantly improve the quality of micro and nano structure of the film. 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 be able to use the current industrialization physical sputtering equipment to further promote the process of industrialization 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 defects, object of the present invention is to provide an apparatus and method using an ion beam sputtering Preparation of micro and nano structure of the film.

[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 film prepared by using micro and nano structures, including ion beam sputtering apparatus and collimating filters, filter device and collimation ion beam sputtering apparatus sample holder connection, collimating filter device comprising: a disk, a number of filters and a plurality of rings, the lower surface of the sample holder disk connection, each ring in turn is superposed on the surface of the disk, the filter disposed in each round 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 disks and rings are provided with openings, disks and rings and fixed by the screw through the openings connected to the sample holder.

[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, number of the rings is two; or in an amount of two filters, 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, the diameter of the disk 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, aperture size of 100 μ m, rib width 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, a 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, disc filters and rings 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 of using an ion beam micro nanostructure film prepared by 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: Preparation of the samples with a photoresist mask polymethyl methacrylate;

[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: Open the ion beam sputtering apparatus main power, filled with nitrogen, open 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 disc collimating filter device, the filter is clamped between the ring and the collimating filter means fixed to the ion beam sputtering apparatus sample holder ;

[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 the vacuum chamber successively sample stage cooling system and mechanical power chestnut, when the degree of vacuum higher than IPa, open molecular chestnut; seriously after the end of the hollow chamber of the 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 then click Close and molecular machinery chestnut chestnut, filled with nitrogen, the sample was removed, the sample was placed in acetone reagent to soak for about five hours to remove the PMMA electron-beam resist, and washed sequentially with acetone, ethanol, and 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, step 4, the ion beam sputtering process parameters:

[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] The deposition time: Cr is 20sec, Ag is 80sec;

[0024] 派射间隔:每派射60sec后间歇5min。 [0024] faction shot interval: 60sec after each shot sent intermittent 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 beneficial effects: the present invention by designing the collimator and filter means disposed in an ion beam sputtering apparatus sample holder, not only can effectively prevent a large angle in oblique incident particles substrate depositing reduce its damaging effects on the photoresist mask (in particular its boundary portion) to produce, and can prevent the deposition produced after the target ion beam bombardment and other large clusters on the substrate, thereby effectively improve preparation the film quality of micro and 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。 For the present invention to expand the physical vapor sputter coating process technology as the core of great significance in the micro and nano structural elements and micro-nano integrated circuit applications in the future.

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] The detailed description is read with reference to non-limiting embodiments with the following drawings, other features of the 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. 1 is a schematic view of the structure of an ion beam apparatus invention Preparation of micro and nano structured thin film sputtered use;

[0028]图2为本发明实施例的准直过滤装置的结构分解图; Structure collimation filter device [0028] Figure 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] Figure 3 is a schematic view of an embodiment of the 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 is adopted before the present invention, the collimator filtration apparatus, after the preparation of micro-nano structure pattern scanning electron microscope (SEM) topography comparison: (a) not to use collimation filter means; (b) to a single-layer filter collimation filter means;

(c)为采用双层过滤网准直过滤装置; (C) the use of double filter collimation 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 for the use of the present invention, the use of double filter collimation micro filtration apparatus array of nanostructures deposited optical topography.

[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, 2 is a collimating filter apparatus, a disk 3, filters 4, 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。 [0033] the following with reference to specific embodiments of the present invention will be described in detail. 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 to further understanding of the present invention, but without limiting the 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, in the present invention without departing from the concept premise, you can also make a number of modifications and improvements. 这些都属于本发明的保护范围。 These are 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] - the kind of use of ion beam sputtering apparatus prepared micro nanostructure film comprising an ion beam sputtering apparatus and collimating filter device 2, the collimator filter device sample holder 2 and the ion beam sputtering apparatus 1 is connected, quasi linear filtering device 2 includes: a disc 3, two filters 4 and three rings 5, and the lower surface of the disc 3 connected to a sample holder, 5 are superposed rings each provided on the surface of the disc 3, filtered net 4 is disposed between the 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 is connected with a sample holder, an upper surface for placing and fixing the sample disc having a diameter of 3 to 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 illustrated, which is a schematic view of the structure of the filter 3. 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。 The filter 4 is slightly larger than the inner diameter of the ring size 5, over the shape of the filter 4 side length 50mm square, the center of the filter diameter of 42mm, a thickness of about 50 μπι, hexagonal mesh structure, the mesh aperture about 100 μm, rib width of about 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] ring disc 5 is not only capable of 3 - from the sample holder fixed to the ion beam sputtering apparatus 1, and between the ring 5 can be tightly sandwiched filter 4. 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 is four inches, an inner diameter of 45mm, a 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 ring disc 5 and 3, respectively, with three holes of 3.5mm diameter are three openings in the circumference of the uniform, respectively, use M3 screws and ring 5 is 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, filters 4 and 5 rings 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] the present example, a double-layered filter collimating 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 a specific number of filters through 4 and 5 of the ring. 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 specific structure of the collimator 2 of filtration apparatus, may be a double filter, the filter can also be a single layer or multi-layer filter, accordingly, the filter 4 and the ring 5 the number may be a filter 4 and two rings 5, or more 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, using the above double-collimating filter is a filtering device 2 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 also provides a method using an ion beam sputtering film prepared by microfabrication of a use, 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 photoresist having a polymethyl methacrylate (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: Open the ion beam sputtering apparatus main power, filled with nitrogen, open 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 disc collimating filter device, the filter is clamped between the ring and the collimating filter means fixed to the ion beam sputtering apparatus sample holder .

[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 the vacuum chamber successively sample stage cooling system and mechanical power chestnut, when the degree of vacuum higher than IPa, open molecular chestnut; seriously after the end of the hollow chamber of the vacuum of 2 * 10 4Pa, open ion beam sputtering 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:

[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] The deposition time: Cr is 20sec, Ag is 80sec;

[0050] 派射间隔:每派射60sec后间歇5min。 [0050] faction shot interval: 60sec after each shot sent intermittent 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, when the filter is not used collimating means, the deposition rate of 4nm / SeC; after adding single collimating filter filtration apparatus, the deposition rate is 2.6nm / sec; added after the double filter collimation filter apparatus, the deposition rate of 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 apparatus embodying the present invention, for the same thickness of film deposition, ion beam sputtering need to pre-calculate the desired time.

[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 then click Close and molecular machinery chestnut chestnut, filled with nitrogen, the sample was removed, the sample was placed in acetone reagent to soak for about five hours to remove the PMMA electron-beam resist and used sequentially with acetone, ethanol, and 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 ion beam deposition of micro and nano structured thin film sputtering technology means below to wide attention for everyone prepared graphene nano-electrode process marker pattern, for example, specify how Si02 (290nm thickness) / Si It is deposited on the substrate thickness of about 40nm micro and nano structure Cr / 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 the side length of about 10mm Si02 / Si substrate sequentially spin-coated on the electron-beam resist 950 and PMMA495 two types, 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) the use of a scanning electron microscope Zeiss Ultra55 and supporting the diaphragm and electron beam pattern generator in which the photoresist mask having (1) exposure of the substrate mark pattern size of 500-1000nm which 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) successively developed in isopropyl alcohol (IPA) and 4-methyl _2_ amyl ketone (MIBK) mixed reagent formulated developer and fixer IPA in 40 seconds and a fixing for 60 seconds and then with nitrogen dry. IPA和MIBK的体积比为3:1。 IPA and MIBK 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, is transferred to the marker pattern 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) turn on the ion beam sputtering apparatus main power, filled with nitrogen, open 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 equipment for the Beijing Institute of Ed Vance ion beam produced LDJ-2A-F100-100 series dual ion beam sputtering deposition 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 prepared in the step of photoresist mask is fixed to the disc-collimating filter device, the filter is then clamped in a single two neighbor samples between a ring (ie, a single filter collimator filtration device), or two filters in turn sandwiched between three rings (ie, dual-filter collimation filter means), and finally this quasi linear filter means is fixed to a sample holder 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) in turn open the vacuum chamber specimen stage cooling system and mechanical power chestnut. 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 higher than IPa, open molecular chestnut; really hollow chamber background vacuum of 2 * 10 4Pa after open ion beam sputtering deposition equipment.

[0060] 离子束溅射工艺中的主要参数如下: [0060] ion beam sputtering process, 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] The deposition time: Cr is 20sec, Ag is 80sec;

[0064] 派射间隔:每派射60sec后间歇5min。 [0064] faction shot interval: 60sec after each shot sent intermittent 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) to calculate the sputtering time, when a sputtering process is complete, click Close and molecular machinery chestnut chestnut, filled 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 was placed in reagent acetone soak for about 5 hours, to remove an electron beam resist PMMA, 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] With the above-described SEM observation of ion beam sputtering apparatus for preparing a metal thin film topography, compared with before the collimation filter means, after the preparation of the topographical variations microfabrication pattern, 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。 We can see, the collimator filtration apparatus of the present invention can significantly improve the quality of the use of ion beam sputter deposition device micro and nano structure of the film. 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。 By ion beam sputtering equipment and the use of double filter shown collimated optical filter structure of micro and nano morphology mark pattern array apparatus of FIG. 5 prepared, you can meet application demands.

[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] The present invention, by an ion beam sputtering apparatus sample holder by means of a collimating filter, can effectively prevent the damaging effects of the oblique incident particle mask (especially the boundary portion) generated and to prevent the ion beam bombard the target produced when wood and other large clusters deposited on the substrate, thereby improving the quality of micro and nano structure of the film, has important applications in the field of nanometer integrated circuits.

[0069] 以上对本发明的具体实施例进行了描述。 [0069] or more specific embodiments of the present invention will be 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。 To be understood that the invention is not limited to the specific embodiments, those skilled in the art can make various changes and modifications within the scope of the claims, this does not affect the substance of the present invention.

Citas de patentes
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Clasificaciones
Clasificación internacionalC23C14/46
Eventos legales
FechaCódigoEventoDescripción
7 Ago 2013C06Publication
20 Nov 2013C10Entry into substantive examination
13 Abr 2016C14Grant of patent or utility model