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CN110060793B - A kind of preparation method of X-ray zone plate - Google Patents

A kind of preparation method of X-ray zone plate Download PDF

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CN110060793B
CN110060793B CN201910367350.4A CN201910367350A CN110060793B CN 110060793 B CN110060793 B CN 110060793B CN 201910367350 A CN201910367350 A CN 201910367350A CN 110060793 B CN110060793 B CN 110060793B
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zone plate
sheet
metal carrier
substrate
ion beam
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CN110060793A (en
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孔祥东
姚广宇
李艳丽
韩立
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Institute of Electrical Engineering of CAS
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    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21KTECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K1/00Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
    • G21K1/06Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diffraction, refraction or reflection, e.g. monochromators
    • G21K1/062Devices having a multilayer structure

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Abstract

The invention discloses a preparation method of an X-ray zone plate, which comprises the following steps: fixing a filament plated with an X-ray zone plate multilayer film structure on a copper sheet, wherein the side surface of the filament is in contact with the copper sheet; fixing the copper sheet on a substrate; cutting the integrated structure of the filaments and the copper sheet into thin sheets; cutting the part of the sheet, which is in contact with the substrate, so that the sheet is completely separated from the substrate; moving and fixing the sheet to a metal carrier web; polishing the thin sheet on the metal carrier net to a required thickness. The invention can ensure that the zone plate is firmly fixed on the metal carrier net and can effectively prevent the zone plate from falling off from the metal carrier net.

Description

一种X射线波带片的制备方法A kind of preparation method of X-ray zone plate

技术领域technical field

本发明涉及波带片制备领域,特别是涉及一种X射线波带片的制备方法。The invention relates to the field of zone plate preparation, in particular to a preparation method of an X-ray zone plate.

背景技术Background technique

X射线波长在0.01-10nm之间,利用X射线波段的显微技术可用于物质的无损检测和三维显微成像,具有对厚样品进行纳米分辨成像的潜力。The X-ray wavelength is between 0.01-10 nm, and the microscopy technology using the X-ray band can be used for non-destructive testing and three-dimensional microscopic imaging of substances, and has the potential to perform nano-resolution imaging of thick samples.

波带片是X射线显微成像技术的核心元件,目前,存在多层膜法制备X射线波带片的技术,即通过溅射的方法在旋转的细丝上交替沉积两种材料,然后将其切成薄片,再将薄片抛光、减薄到所要求的厚度。采用该工艺制备的X射线波带片是一个直径为几微米到几百微米、厚度一般为亚10微米的圆形薄片,现有的波带片固定方法中一般是采用聚焦离子束沉积工艺将波带片与载网等固定在一起。但由于波带片为圆形结构,波带片仅在与载网相切的部分相接触,接触面非常小,固定后的粘合力较弱,难于抵抗稍强的冲击力,在操作过程中很容易被损坏或丢失。The zone plate is the core component of X-ray microscopy imaging technology. At present, there is a technology for preparing X-ray zone plates by the multilayer film method, that is, two materials are alternately deposited on the rotating filament by sputtering, and then the It is cut into thin slices, which are polished and thinned to the desired thickness. The X-ray zone plate prepared by this process is a circular slice with a diameter of several microns to several hundreds of microns and a thickness of generally sub-10 microns. The zone plate is fixed with the carrier net and the like. However, due to the circular structure of the zone plate, the zone plate is only in contact with the tangent part of the carrier network, the contact surface is very small, the adhesion after fixing is weak, and it is difficult to resist slightly stronger impact force. can easily be damaged or lost.

发明内容SUMMARY OF THE INVENTION

本发明的目的是提供一种X射线波带片的制备方法,增强波带片和金属载网之间的粘合力,使得波带片能够很稳固地置于金属载网之上,提高波带片抵抗冲击力的能力。The purpose of the present invention is to provide a preparation method of an X-ray zone plate, which can enhance the adhesion between the zone plate and the metal carrier net, so that the wave zone plate can be placed on the metal carrier net very stably, and the wave The ability of the strap to resist impact forces.

为实现上述目的,本发明提供了如下方案:For achieving the above object, the present invention provides the following scheme:

一种X射线波带片的制备方法,包括:A preparation method of an X-ray zone plate, comprising:

将镀有X射线波带片多层膜结构的细丝固定于铜皮上,所述细丝的侧表面与所述铜皮接触;Fixing the filament coated with the multi-layer film structure of the X-ray zone plate on the copper skin, and the side surface of the filament is in contact with the copper skin;

将载有所述细丝的铜皮固定于衬底上;fixing the copper skin carrying the filaments on the substrate;

将所述细丝和铜皮的一体结构切割成薄片;cutting the integrated structure of the filament and the copper skin into thin slices;

切割所述薄片与衬底接触的部分,使所述薄片完全脱离所述衬底;cutting the part of the sheet in contact with the substrate, so that the sheet is completely separated from the substrate;

将所述薄片移动并固定到金属载网上;moving and securing the sheet to the metal carrier grid;

将所述金属载网上的薄片抛光成所需厚度。The flakes on the metal carrier are polished to the desired thickness.

可选的,所述细丝通过液体碳胶固定于所述铜皮上。Optionally, the filaments are fixed on the copper skin by liquid carbon glue.

可选的,所述铜皮厚度小于10微米。Optionally, the thickness of the copper skin is less than 10 microns.

可选的,所述铜皮通过导电胶固定于所述衬底上。Optionally, the copper skin is fixed on the substrate by conductive glue.

可选的,采用聚焦离子束将所述细丝和铜皮的一体结构切割成薄片。Optionally, a focused ion beam is used to cut the integrated structure of the filament and the copper skin into thin slices.

可选的,采用聚焦离子束切割所述薄片的与衬底接触的部分,使所述薄片完全脱离所述衬底。Optionally, a focused ion beam is used to cut the portion of the sheet in contact with the substrate, so that the sheet is completely separated from the substrate.

可选的,将机械臂固定于所述薄片外表面并采用聚焦离子束切割所述薄片的与衬底接触的部分,使所述薄片完全脱离所述衬底。Optionally, a robotic arm is fixed on the outer surface of the sheet and a focused ion beam is used to cut the portion of the sheet in contact with the substrate, so that the sheet is completely separated from the substrate.

可选的,使用机械臂将所述薄片移动到金属载网上,采用聚焦离子束沉积技术将所述薄片固定到所述金属载网上,然后移去所述机械臂。Optionally, a robotic arm is used to move the sheet onto the metal carrier, the sheet is fixed on the metal carrier by a focused ion beam deposition technique, and then the robotic arm is removed.

可选的,采用聚焦离子束将所述金属载网上的薄片抛光成所需厚度。Optionally, a focused ion beam is used to polish the flakes on the metal carrier to a desired thickness.

根据本发明提供的具体实施例,本发明公开了以下技术效果:According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects:

本发明将波带片与铜皮之间通过液体碳胶相粘合,粘合面积和粘合力远大于波带片与金属载网直接连接,且铜皮与金属载网的接触是平面接触,接触面积较大,使得波带片能够很稳固地置于金属载网之上,能够抵抗较强的冲击力,另外,附带上铜皮的波带片尺寸已经在几个毫米量级,完全能够凭借宏观的手段进行移动和安装,能够有效提高安装效率和安装精确度。In the invention, the zonal sheet and the copper skin are bonded by liquid carbon glue, and the bonding area and the bonding force are much larger than the direct connection between the zonal sheet and the metal carrier net, and the contact between the copper sheet and the metal carrier net is plane contact, The contact area is large, so that the zone plate can be placed on the metal carrier network firmly and can resist strong impact. Moving and installing by means of macro can effectively improve installation efficiency and installation accuracy.

附图说明Description of drawings

为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the accompanying drawings required in the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some of the present invention. In the embodiments, for those of ordinary skill in the art, other drawings can also be obtained according to these drawings without creative labor.

图1为本发明实施例一种X射线波带片的制备方法的工作流程图;Fig. 1 is a working flow diagram of a method for preparing an X-ray zone plate according to an embodiment of the present invention;

图2为根据本发明实施例一种X射线波带片的制备方法得到的波带片结构示意图;2 is a schematic structural diagram of a zone plate obtained by a method for preparing an X-ray zone plate according to an embodiment of the present invention;

1-金属载网,2-波带片,3-液体碳胶,4-铜皮。1- Metal carrier net, 2- Zone plate, 3- Liquid carbon glue, 4- Copper skin.

具体实施方式Detailed ways

下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

本发明的目的是提供一种X射线波带片的制备方法,增强波带片和金属载网之间的粘合力,使得波带片能够很稳固地置于金属载网之上,提高波带片抵抗冲击力的能力。The purpose of the present invention is to provide a preparation method of an X-ray zone plate, which can enhance the adhesion between the zone plate and the metal carrier net, so that the wave zone plate can be placed on the metal carrier net very stably, and the wave The ability of the strap to resist impact forces.

为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合附图和具体实施方式对本发明作进一步详细的说明。In order to make the above objects, features and advantages of the present invention more clearly understood, the present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments.

图1为本发明实施例工作流程图,如图1所示,一种X射线波带片的制备方法,包括:Fig. 1 is a working flowchart of an embodiment of the present invention. As shown in Fig. 1, a preparation method of an X-ray zone plate includes:

101将镀有X射线波带片多层膜结构的细丝固定于铜皮上,所述细丝的侧表面与所述铜皮接触;101 Fix the filament coated with the multi-layer film structure of the X-ray zone plate on the copper skin, and the side surface of the filament is in contact with the copper skin;

102将载有所述细丝的铜皮固定于衬底上;102 fixing the copper skin carrying the filament on the substrate;

103将所述细丝和铜皮的一体结构切割成薄片;103 cutting the integrated structure of the filament and the copper skin into thin slices;

104切割所述薄片与衬底接触的部分,使所述薄片完全脱离所述衬底;104 cutting the part of the sheet in contact with the substrate, so that the sheet is completely separated from the substrate;

105将所述薄片移动并固定到金属载网上;105 moving and securing the sheet to the metal carrier grid;

106将所述金属载网上的薄片抛光成所需厚度。106 The flakes on the metal carrier are polished to the desired thickness.

其中,所述细丝通过液体碳胶固定于所述铜皮上,细丝的直径为几微米到几百微米;所述铜皮两端通过导电胶固定于所述衬底上,铜皮的厚度一般小于10微米;衬底材料可为任意表面光滑的导体或半导体片状材料。Wherein, the filament is fixed on the copper skin by liquid carbon glue, and the diameter of the filament is several microns to several hundreds of microns; both ends of the copper skin are fixed on the substrate by conductive glue, and the copper skin is The thickness is generally less than 10 microns; the substrate material can be any smooth-surfaced conductor or semiconductor sheet material.

具体的,该方法采用聚焦离子束(FIB)将所述细丝和铜皮的一体结构切割成略大于所需厚度的薄片;然后将机械臂固定于所述薄片外表面并采用聚焦离子束切割所述薄片与衬底接触的部分,使所述薄片能够完全脱离衬底;再使用机械臂将所述薄片移动到金属载网上,采用聚焦离子束沉积技术将所述薄片固定到所述金属载网上,然后移去所述机械臂;最后采用聚焦离子束将所述金属载网上的薄片抛光成所需厚度即可,其中,所需厚度一般为亚10微米。Specifically, the method uses a focused ion beam (FIB) to cut the integrated structure of the filament and the copper skin into a thin sheet with a thickness slightly larger than the required thickness; then the robotic arm is fixed on the outer surface of the thin sheet and the focused ion beam is used to cut The part of the sheet in contact with the substrate enables the sheet to be completely separated from the substrate; then use a robotic arm to move the sheet to the metal carrier net, and use the focused ion beam deposition technology to fix the sheet on the metal carrier Then, the robotic arm is removed; finally, a focused ion beam is used to polish the sheet on the metal carrier net to a desired thickness, wherein the desired thickness is generally sub-10 microns.

图2为根据本发明实施例一种X射线波带片的制备方法得到的波带片结构示意图,如图2所示,其中,所述波带片2通过液体碳胶3固定于铜皮4上,所述铜皮4通过聚焦离子束沉积技术固定到所述金属载网1上。FIG. 2 is a schematic structural diagram of a zone plate obtained by a method for preparing an X-ray zone plate according to an embodiment of the present invention, as shown in FIG. 2 , wherein the zone plate 2 is fixed on a copper skin 4 by a liquid carbon glue 3 Above, the copper skin 4 is fixed on the metal carrier mesh 1 by the focused ion beam deposition technology.

本发明还公开了如下技术效果:The present invention also discloses the following technical effects:

1.本发明将波带片与铜皮之间通过液体碳胶相粘合,粘合面积和粘合力远大于波带片与载网直接连接;且铜皮与载网的接触是平面接触,接触面积较大,使得波带片能够很稳固地置于载网之上,强能够抵抗较强的冲击力,可以有效防止波带片从金属载网上脱落。1. The present invention bonds between the wave zone sheet and the copper skin through the liquid carbon glue, and the bonding area and the adhesive force are far greater than the direct connection between the wave zone sheet and the carrier screen; and the contact between the copper sheet and the carrier screen is a plane contact, The large contact area enables the zone plate to be placed on the carrier network very stably, can resist strong impact force, and can effectively prevent the zone plate from falling off the metal carrier network.

2.本发明附带铜皮的波带片尺寸已经在几个毫米量级,完全可以凭借宏观的手段进行移动和安装,可以有效提高安装效率和安装精确度。2. The size of the wave zone plate with copper skin in the present invention is already in the order of several millimeters, and it can be moved and installed by means of macroscopic methods, which can effectively improve the installation efficiency and installation accuracy.

本说明书中各个实施例采用递进的方式描述,每个实施例重点说明的都是与其他实施例的不同之处,各个实施例之间相同相似部分互相参见即可。The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments, and the same and similar parts between the various embodiments can be referred to each other.

本文中应用了具体个例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其核心思想;同时,对于本领域的一般技术人员,依据本发明的思想,在具体实施方式及应用范围上均会有改变之处。综上所述,本说明书内容不应理解为对本发明的限制。In this paper, specific examples are used to illustrate the principles and implementations of the present invention. The descriptions of the above embodiments are only used to help understand the methods and core ideas of the present invention; meanwhile, for those skilled in the art, according to the present invention There will be changes in the specific implementation and application scope. In conclusion, the contents of this specification should not be construed as limiting the present invention.

Claims (5)

1. A method of making an X-ray zone plate, comprising:
fixing a filament plated with an X-ray zone plate multilayer film structure on a copper sheet through liquid carbon gel, wherein the side surface of the filament is in contact with the copper sheet;
fixing two ends of the copper sheet carrying the filaments on a substrate through conductive adhesive;
cutting the integrated structure of the filaments and the copper sheets into thin sheets by adopting a focused ion beam;
cutting the part of the thin sheet, which is contacted with the substrate, by using a focused ion beam to ensure that the thin sheet is completely separated from the substrate;
moving the thin sheet and fixing the thin sheet on a metal carrying net by adopting a focused ion beam deposition technology;
polishing the thin sheet on the metal carrier net to a required thickness.
2. A method of manufacturing an X-ray zone plate according to claim 1, wherein the copper sheet is less than 10 microns thick.
3. A method of manufacturing an X-ray zone plate according to claim 1, wherein a robotic arm is fixed to the outer surface of the lamella.
4. A method of manufacturing an X-ray zone plate according to claim 1, wherein the wafer is moved onto a metal carrier using a robot arm, the wafer is fixed onto the metal carrier using a focused ion beam deposition technique, and the robot arm is removed.
5. A method of manufacturing an X-ray zone plate according to claim 1, wherein the sheet on the metal carrier mesh is polished to a desired thickness using a focused ion beam.
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CN110441115B (en) * 2019-09-09 2022-02-22 中国科学院电工研究所 Preparation method of multilayer film X-ray zone plate

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