WO2020010522A1 - 一种独立金属薄膜制备方法及金属薄膜 - Google Patents

一种独立金属薄膜制备方法及金属薄膜 Download PDF

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Publication number
WO2020010522A1
WO2020010522A1 PCT/CN2018/095163 CN2018095163W WO2020010522A1 WO 2020010522 A1 WO2020010522 A1 WO 2020010522A1 CN 2018095163 W CN2018095163 W CN 2018095163W WO 2020010522 A1 WO2020010522 A1 WO 2020010522A1
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Prior art keywords
thin film
metal thin
transfer coating
substrate
metal
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PCT/CN2018/095163
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English (en)
French (fr)
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龚国华
何江
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深圳通感微电子有限公司
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Priority to PCT/CN2018/095163 priority Critical patent/WO2020010522A1/zh
Publication of WO2020010522A1 publication Critical patent/WO2020010522A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering

Definitions

  • the invention relates to the technical field of metal thin film preparation, and more particularly, to a method for preparing an independent metal thin film and a metal thin film.
  • the technical problem to be solved by the present invention is to provide a method for preparing an independent metal thin film and a metal thin film in response to the foregoing technical defects of the prior art.
  • the technical solution adopted by the present invention to solve its technical problems is to construct a method for preparing an independent metal thin film, including the following steps:
  • a metal material is selected and deposited on the surface of the cured transfer coating to generate a metal film of a preset thickness; the deposition includes:
  • the thickness of the transfer coating is 0.5-2 times the preset thickness of the metal thin film.
  • the substrate temperature does not exceed 80 ° C.
  • the filling argon under vacuum includes filling argon to a pressure of 0.4-4Pa.
  • the preset thickness of the metal thin film is 50-1000 nm.
  • the surface flatness of the substrate is ⁇ 10 nm.
  • the metal material is one or more of Au, Ag, Cu, Cr, Al, Ni, and Ti.
  • the transferring process includes using a mesh structure or a hollow ring frame tool to lift the metal thin film to keep the metal thin film in an unfolded state.
  • step S2 the following steps are further performed:
  • Preset pattern A preset pattern is set on the surface of the solidified transfer coating.
  • the invention also constructs a metal thin film, which is obtained by any of the independent metal thin film preparation methods described above.
  • the method for preparing the independent metal thin film and the metal thin film of the present invention have the following beneficial effects: the preparation of the independent metal thin film that meets the requirements can be obtained, the method is simple and easy, and the cost is low.
  • FIG. 1 is a schematic flowchart of a first embodiment of a method for preparing an independent metal thin film according to the present invention
  • FIG. 2 is a schematic process diagram of a first embodiment of a method for preparing an independent metal thin film according to the present invention
  • FIG. 3 is a schematic flowchart of a second embodiment of a method for preparing an independent metal thin film according to the present invention.
  • FIG. 4 is a schematic process diagram of a second embodiment of a method for preparing an independent metal thin film according to the present invention.
  • a transfer coating selecting a substrate whose surface satisfies optical level flatness, and The substrate is cleaned and dried, and a transfer coating is spin-coated on the surface of the substrate. Specifically, the substrate is cleaned and dried with an optical level flatness that meets the requirements to ensure the surface is clean and dry.
  • the substrate here can be silicon or silicon. Glass and similar materials.
  • a conventional photoresist spin coater is used to spin-coat a transfer coating with a thickness of 100 to 1000 nm.
  • the transfer coating here can be PMMA or photoresist.
  • PMMA is used.
  • the properties of PMMA after curing are relatively stable. Compared with silicone oil, molten metals, or liquid crystal materials, PMMA is easier to obtain, lower in cost, and does not volatilize during the deposition of metal thin films. Will affect or pollute the vacuum environment.
  • the thickness of PMMA can be controlled by the speed of the spin coater and the viscosity of PMMA.
  • the viscosity of PMMA can be controlled by the ratio of PMMA to the solvent.
  • the solvent here can be phenol or anisole.
  • Deposition Select a metal material to deposit on the surface of the solidified transfer coating to generate a metal film of a predetermined thickness.
  • Deposition includes: filling argon under vacuum and depositing metal on the surface of the transfer coating by a sputtering power source. Thin film; or metal materials are heated and vaporized by an electron beam power source under vacuum to deposit a metal thin film on the surface of the transfer coating; specifically, the spin-coated PMMA substrate is placed in a vacuum chamber, where The atmospheric pressure satisfied by the vacuum chamber is 10 -4 Pa or less.
  • Deposition is performed on the surface of the transfer coating under vacuum conditions to generate a metal film of a predetermined thickness. In addition, during the metal film deposition process, the thickness of the film can be monitored using crystal oscillator technology.
  • metal thin film deposition can be as follows: select the required metal material target (Au, Ag, Pt, Cr, Ti, Al, etc.) and install it on the target base, put the PMMA substrate spin-coated, and place
  • the atmospheric pressure of the vacuum chamber is maintained below 10 -4 Pa, and no impurity gas is guaranteed during the film deposition process. Filled with high-purity argon, the pressure inside the cavity can be maintained between 0.4-4Pa, and the pressure can be kept stable.
  • the sputtering power the sputtering current is maintained at 0.1-0.5A, the sputtering voltage is 220-550V, and the argon plasma is excited.
  • a metal thin film deposition process may also be employed the following specific actions: selecting the desired powder metal material is placed in the evaporation crucible, placed in a good spin-coating PMMA substrate, the background vacuum chamber was evacuated to 10-4-10-- Below 5 Pa, it is guaranteed that there are no other impurity gases under vacuum conditions during metal film deposition. Turn on the power of the electron beam, maintain its output power at 800-3000W, and excite the electron beam to heat and vaporize the metal material in the crucible, so that the metal material is deposited on the substrate.
  • the atmospheric pressure is controlled during the metal thin film deposition process.
  • the air pressure is low.
  • the metal thin film deposition rate will be slow, so the grains of the metal thin film will be smaller, and the internal stress of the metal thin film will be smaller. It is beneficial to the peeling of the metal film and is not brittle.
  • the particle size of the metal film is too large, the internal stress of the metal film will be relatively large. In this way, the metal film is relatively easy to break during the peeling process of the metal film, so it is assured during the metal film deposition process. Its low pressure vacuum environment.
  • the substrate with the metal film is placed in an organic solvent that can dissolve the transfer coating at normal temperature to separate the metal film.
  • the organic solvent here is a solvent that can dissolve the transfer coating without damaging the substrate and the metal thin film.
  • the substrate and the metal film are not affected by the solvent.
  • the transfer coating is PMMA
  • the organic solvent may be acetone.
  • the temperature must be maintained at normal temperature, for example, the temperature is controlled at 25 ⁇ 5 ° C until the metal thin film is completely separated from the substrate.
  • 300 nm Ag is peeled off.
  • the relative molecular mass of PMMA is 50 K and the thickness is 300 nm. The metal film and the substrate can be easily and naturally separated.
  • the thickness of the transfer coating layer is 0.5-2 times the preset thickness of the metal thin film. Specifically, in order to ensure that the thickness of the finally obtained metal film meets the requirements, the thickness of the transfer coating usually meets the target thickness of the metal film by 0.5-2 times. In this way, the quality of the metal film and the quality of the metal film during the deposition process can be guaranteed. The integrity of the metal film is ensured during the subsequent metal film peeling process, that is, the deposited metal film will not be easily broken. In addition, the peeling process of the metal thin film is simplified, which reduces waste of time and materials.
  • step S3 during the process of depositing on the surface of the solidified transfer coating to form a metal film with a predetermined thickness, the substrate temperature does not exceed 80 ° C. Specifically, at the same time, the temperature of the substrate is monitored during the metal thin film deposition process to ensure that the temperature of the substrate does not exceed 80 ° C. When the temperature exceeds 80 ° C, the electron beam power source or the sputtering power source is stopped to stop the metal thin film. Deposition.
  • the stress of the metal thin film should be controlled during the deposition of the metal thin film.
  • the temperature of the substrate changes greatly during the deposition of the metal thin film, the stress of the metal thin film formed by the deposition will increase, and the metal thin film is easily broken during the peeling process. So controlling the substrate temperature is also a key element.
  • filling argon under vacuum includes filling argon to a pressure of 0.4-4Pa.
  • the ambient air pressure has an impact on the grain structure and stress of the metal thin film.
  • the argon gas can satisfy the metal
  • the argon gas pressure environment can satisfy 0.4-4Pa.
  • the gold (Au) film maintained at a vacuum of 0.4 Pa during metal film deposition is more likely to peel off, and the peeled metal film is more likely to maintain integrity.
  • the preset thickness of the metal thin film is 50-1000 nm.
  • the crystal film technology can be used to monitor the thickness of the film, so that the thickness of the final metal thin film can meet 50-1000 nm, so as to ensure easier stripping of the metal thin film and ensure its integrity during the stripping process. .
  • the surface flatness of the substrate is ⁇ 10 nm / cm 2 , and the property does not change at a temperature of 180 ° C.
  • the flatness of the substrate surface is controlled to ensure that the flatness of the spin-coated transfer coating can meet the requirements, and finally the flatness of the obtained metal film can meet the requirements
  • the metal material is one or more of Au, Ag, Cu, Cr, Al, Ni, and Ti.
  • the metal material may be any one of gold (Au), silver (Ag), platinum (Pt), copper (Cu), chromium (Cr), titanium (Ti), iron (Fe), and nickel (Ni).
  • gold Au
  • silver Ag
  • platinum Pt
  • copper Cu
  • Cr chromium
  • titanium Ti
  • iron Fe
  • Ni nickel
  • Ni nickel
  • the transfer process includes using a mesh structure or a hollow ring frame tool to lift the metal thin film to keep the metal thin film in an unfolded state.
  • the metal thin film is suspended in the solution after being separated from the substrate.
  • a hollow ring frame or mesh structured tool can be used to hold the metal film from below, so that the metal film remains unfolded on the surface of the hollow ring frame or meshed tool, and the hollow and mesh structure can The solution is filtered off, so that the transfer of the metal film is very important.
  • Preset pattern A preset pattern is set on the surface of the solidified transfer coating. Specifically, a corresponding mold can be used to emboss the top surface of the spin-coated transfer coating to make the final metal thin film form the final required pattern. It can be understood here that the pattern on the transfer coating is opposite to the pattern of the final metal thin film.
  • the independent metal thin film material with a specific surface shape can be processed according to needs, and is not limited to making a flat independent metal thin film.
  • the metal material is heated and vaporized by the electron beam power source under vacuum conditions to deposit and generate a metal thin film on the surface of the transfer coating layer to better achieve step coverage and micro-hole coverage of large and deep pores. .
  • the thermal stress of the metal film is small, and the metal film can maintain better toughness, so that Not easy to crack during use. And it can effectively peel out a whole 3D structure metal thin film material with a thickness of tens to hundreds of nanometers.
  • an independent metal thin film having a large area can be formed, and the area of the independent metal thin film can be up to 10 cm * 10 cm.
  • the metal thin film of the present invention can be prepared by the above-mentioned partial method. According to the above method for preparing an independent metal thin film, an independent metal thin film finally required can be prepared, and more usage scenarios are also satisfied.
  • the metal film obtained by the above method has low thermal stress, can maintain better toughness of the metal film, and is not easily broken during use.

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Abstract

一种独立金属薄膜制备方法及金属薄膜，该方法包括：S1、旋涂转移涂层：选择表面满足光学级平整度的衬底，对衬底进行清洗烘干并在衬底表面上旋涂转移涂层；S2、固化：蒸发并冷却旋涂转移涂层后的衬底，以固化转移涂层；S3、沉积：选用金属材料，在固化的转移涂层表面沉积以生成预设厚度的金属薄膜；S4、剥离：在常温下将带有金属薄膜的衬底置于可溶解转移涂层的有机溶剂中，以分离金属薄膜；S5、转移：保持金属薄膜为展开状态并转移金属薄膜至无氧条件下烘干，以得到最终的独立金属薄膜。该技术方案能够获取满足要求的独立金属薄膜制备，方法简单易行，且成本低。

Description

一种独立金属薄膜制备方法及金属薄膜 技术领域
本发明涉及金属薄膜制备技术领域，更具体地说，涉及一种独立金属薄膜制备方法及金属薄膜。
 背景技术
在科学研究和实际半导体工艺中常常会用到厚度为几十到几百纳米的悬空薄膜，这种薄膜由于太薄不宜剥离，因此很难采用常规方法制备。
 技术问题
本发明要解决的技术问题在于，针对现有技术的上述技术缺陷，提供一种独立金属薄膜制备方法及金属薄膜。
 技术解决方案
本发明解决其技术问题所采用的技术方案是：构造一种独立金属薄膜制备方法，包括以下步骤：
S1、旋涂转移涂层：选择表面满足光学级平整度的衬底，对所述衬底进行清洗烘干并在所述衬底表面上旋涂转移涂层；
S2、固化：蒸发并冷却旋涂所述转移涂层后的衬底，以固化所述转移涂层；
S3、沉积：选用金属材料，在固化的转移涂层表面沉积以生成预设厚度的金属薄膜；所述沉积包括：
在真空条件下充入氩气，并通过溅射电源在所述转移涂层表面沉积生成所述金属薄膜；或
在真空条件下通过电子束电源对所述金属材料加热气化，以在所述转移涂层表面沉积生成所述金属薄膜；
S4、剥离：在常温下将带有所述金属薄膜的衬底置于可溶解所述转移涂层的有机溶剂中，以分离所述金属薄膜；
S5、转移：保持所述金属薄膜为展开状态并转移所述金属薄膜至无氧条件下烘干，以得到最终的独立金属薄膜。
优选地，在所述步骤S1中，所述在所述衬底表面上旋涂转移涂层过程中，所述转移涂层厚度为所述金属薄膜的预设厚度的0.5-2倍。
优选地，在所述步骤S3中，在所述在固化的转移涂层表面沉积以生成预设厚度的金属薄膜过程中，所述衬底温度不超过80℃。
优选地，在所述步骤S3中，所述在真空条件下充入氩气包括：充入氩气至气压满足0.4-4Pa。
优选地，在所述步骤S3中，所述金属薄膜的预设厚度为50-1000nm。
优选地，在所述步骤S1中，所述衬底的表面平整度为±10nm。
优选地，在所述步骤S3中，所述金属材料为Au、Ag、Cu、Cr、Al、Ni、Ti中的一种或多种。
优选地，在所述步骤S5中，所述转移过程包括，使用网状结构或中空的环形框工具对所述金属薄膜进行托举以保持所述金属薄膜为展开状态。
优选地，在所述步骤S2后，还执行以下步骤：
S2-1、预设图案：在固化后的转移涂层表面设置预设图案。
本发明还构造一种金属薄膜，通过上面任意所述的独立金属薄膜制备方法制备获取。
 有益效果
实施本发明的独立金属薄膜制备方法及金属薄膜，具有以下有益效果：能够获取满足要求的独立金属薄膜制备，方法简单易行，且成本低。
 附图说明
下面将结合附图及实施例对本发明作进一步说明，附图中：
图1是本发明一种独立金属薄膜制备方法第一实施例的流程示意图；
图2是本发明一种独立金属薄膜制备方法第一实施例的过程示意图；
图3是本发明一种独立金属薄膜制备方法第二实施例的流程示意图；
图4是本发明一种独立金属薄膜制备方法第二实施例的过程示意图。
 本发明的实施方式
为了对本发明的技术特征、目的和效果有更加清楚的理解，现对照附图详细说明本发明的具体实施方式。
如图1和图2所示，在本发明的一种独立金属薄膜制备方法第一实施例中，包括以下步骤：S1、旋涂转移涂层：选择表面满足光学级平整度的衬底，对衬底进行清洗烘干并在衬底表面上旋涂转移涂层；具体的，取表面光学级平整度满足要求的衬底清洗烘干，保证表面洁净、干燥；这里的衬底可以选择硅或者玻璃等类似材。在处理干净的衬底表面采用常规光刻胶旋涂机旋涂厚度为100~1000nm的转移涂层，这里的转移涂层可以采用PMMA或光刻胶等。在这里的实施例中，采用PMMA， PMMA固化后性质较为稳定，与相对于硅油、熔融的金属或液晶材料相比，PMMA易获得，成本低，并且在金属薄膜沉积过程中不会挥发，不会对真空环境产生影响或污染。在旋涂过程中，PMMA厚度可以通过旋涂机转速和PMMA黏度来控制，PMMA黏度可以通过PMMA与溶剂比例来控制，这里的溶剂可以采用苯酚或者苯甲醚等。
S2、固化：蒸发并冷却旋涂转移涂层后的衬底，以固化转移涂层；具体的，将将旋涂好PMMA的衬底放置于烘干炉上蒸发以去掉溶剂，然后冷却固化该PMMA，使衬底上的转移涂层为硬质结构。
S3、沉积：选用金属材料，在固化的转移涂层表面沉积以生成预设厚度的金属薄膜；沉积包括：在真空条件下充入氩气，并通过溅射电源在转移涂层表面沉积生成金属薄膜；或在真空条件下通过电子束电源对金属材料加热气化，以在转移涂层表面沉积生成金属薄膜；具体的，将旋涂好的PMMA的衬底放置于真空腔体中，这里的真空腔体满足的大气压为10 -4Pa以下。在真空条件上在转移涂层表面进行沉积，生成预设厚度的金属薄膜，此外，在金属薄膜沉积过程中可采用用晶振片技术来实施监测薄膜厚度。这里金属薄膜的沉积的具体操作可以为：选择所需金属材料靶材（Au、Ag、Pt、Cr、Ti、Al等）并安装至靶座上，放入旋涂好PMMA的衬底，将真空腔体大气压维持在10 -4Pa以下，并保证薄膜沉积过程中无杂质气体。充入高纯氩气，在这里可以使充入氩气后的腔体内气压维持在0.4-4Pa之间，并维持气压稳定。打开溅射电源，溅射电流维持在0.1-0.5A，溅射电压220-550V，激发氩气等离子体。等离子体中氩气+轰击金属靶材表面，溅射出金属原子沉积到衬底上形成金属薄膜。金属薄膜沉积的过程还可以采用如下的具体操作：选择所需金属材料粉末放置于蒸发坩埚中，放入旋涂好PMMA的衬底，将真空腔体本底真空抽至10 -4-10 -5Pa以下，保证在金属薄膜沉积过程中真空条件下无其他杂质气体。打开电子束电源，维持其输出功率在800-3000W，激发电子束对坩埚内的金属材料进行加热并气化，使金属材料沉积在衬底上。此外，在金属薄膜沉积过程中控制环境气压，是气压位置较低状态，当气压低时，金属薄膜的沉积速度会慢，这样金属薄膜的晶粒会小些，金属薄膜内应力会小，这样有利于金属薄膜的剥离而不易碎，当金属薄膜的颗粒太大，金属薄膜内应力会比较大，这样在金属薄膜的剥离过程中，金属薄膜相对容易破碎，所以在金属薄膜沉积过程中尽量保证其低气压真空环境。
S4、剥离：在常温下将带有金属薄膜的衬底置于可溶解转移涂层的有机溶剂中，以分离金属薄膜；具体的，将沉积形成预设厚度的金属薄膜的衬底浸泡于有机溶剂中，这里的有机溶剂是可以溶解该转移涂层、且不破坏衬底和金属薄膜的溶剂。这样在有机溶剂溶解转移涂层的过程中经，衬底和金属薄膜不受溶剂影响。例如当转移涂层为PMMA时，有机溶剂可以采用丙酮。此外在溶剂溶剂转移涂层的过程中，要保证温度为常温，例如温度控制在25±5℃，直至金属薄膜与衬底完全分离。此外这里要说明的是，PMMA相对分子质量越小，在其表面形成的金属薄膜越易剥离，例如剥离300nmAg，采用PMMA相对分子质量为50K、厚度为300nm,在25℃的丙酮中维持30min，金属薄膜和衬底会很容易的自然分离。
S5、转移：保持金属薄膜为展开状态并转移金属薄膜至无氧条件下烘干，以得到最终的独立金属薄膜。具体的，在金属薄膜与衬底分离后，金属薄膜会悬浮于溶液中，而金属薄膜使用中必然存在对金属薄膜的专利过程，这里金属薄膜转移过程中要保证金属薄膜一直为展开状态，同时将取出的金属薄膜置于无氧条件烘干，这样得到最终的独立金属薄膜，供各种需要的场景使用。这里的无氧条件可以为将金属薄膜从溶液中取出后，置于氮气箱中烘干。当然这里的无氧环境不局限于上面描述。
进一步的，在步骤S1中，在衬底表面上旋涂转移涂层过程中，转移涂层厚度为金属薄膜的预设厚度的0.5-2倍。具体的，为了保证最后获得的金属薄膜的厚度满足要求，通常在转移涂层的厚度满足金属薄膜的目标厚度的0.5-2倍，这样，可以保证金属薄膜的沉积过程中，金属薄膜的质量和后面金属薄膜剥离过程中保证金属薄膜的完整，即沉积的金属薄膜不会容易碎裂。此外也使金属薄膜的剥离过程简单，减少时间和材料的浪费。
进一步的，在步骤S3中，在在固化的转移涂层表面沉积以生成预设厚度的金属薄膜过程中，衬底温度不超过80℃。具体的，同时在金属薄膜沉积过程中对衬底的温度进行实施监测，保证衬底的温度不超过80℃，当出现超过80℃时，停止电子束电源或者溅射电源，以停止金属薄膜的沉积。这里在金属薄膜的沉积过程中要控制金属薄膜应力，当金属薄膜沉积过程中，衬底的温度变化大，沉积形成的金属薄膜应力会增加，那么金属薄膜在其剥离过程中容易碎裂。所以控制衬底温度也是一个关键的要素。
进一步的，在真空条件下充入氩气包括：充入氩气至气压满足0.4-4Pa。具体的，如前面描述，在金属薄膜沉积过程中，环境气压对生成金属薄膜的晶粒结构及应力有影响，这样在真空环境中充入氩气气体时，要保证充入氩气能够满足金属薄膜沉积过程的需要，且同时保证生成的金属薄膜的晶粒结构及应力满足金属薄膜剥离过程的需要，这样在充入氩气的过程中，使充入氩气的气压环境满足0.4-4Pa。此外，可以了解到，在金属薄膜沉积过程中真空度维持0.4Pa下的金（Au）薄膜更容易剥离，并且剥离的金属薄膜更容易保持完整性。
进一步的，在步骤S3中，金属薄膜的预设厚度为50-1000nm。具体的，在金属薄膜沉积过程中可采用晶振片技术来实施监测薄膜厚度，以使最终金属薄膜的厚度满足50-1000nm，以便保证金属薄膜的更容易剥离且保证其在剥离过程中的完整性。
进一步的，，在步骤S1中，衬底的表面平整度为±10nm/cm 2，温度在180℃性质不发生变化。具体的，控制衬底表面的平整度，以保证其表面旋涂的转移涂层的平整度能够满足要求，最终是获取到的金属薄膜的平整度能够满足要求
进一步的，在步骤S3中，金属材料为Au、Ag、Cu、Cr、Al、Ni、Ti中的一种或多种。具体的，金属材料可以为金（Au）、银（Ag）、铂（Pt）、铜（Cu）、铬（Cr）、钛（Ti）、铁（Fe）、镍（Ni）中的任意一种，也可以为多种，例如为多种金属材料组成的合金。
进一步的，在步骤S5中，转移过程包括，使用网状结构或中空的环形框工具对金属薄膜进行托举以保持金属薄膜为展开状态。具体的，金属薄膜与衬底分离后会悬浮于溶液中，此时若直接取出金属薄膜，金属薄膜很容易缠结一起。因此，这里可以采用中空的环形框或网状结构的工具从下面托住金属薄膜，这样金属薄膜在中空的环形框或网状结构的工具的表面保持为展开状态，且中空和网状结构可以使溶液滤除，这样就很方面金属薄膜的转移。
如图3和图4所示，在所述步骤S2后，还执行以下步骤：S2-1、预设图案：在固化后的转移涂层表面设置预设图案。具体的，可以利用相对应的模具在旋涂好的转移涂层上表面压印，以使最终的金属薄膜形成最终的需要的图形。这里可以理解，在转移涂层上的图案与最终的金属薄膜的图案为相反图案。可以根据需要加工出特定表面形状的独立金属薄膜材料，而不局限于制作平整的独立金属薄膜。此外，在这里，通过在真空条件下通过电子束电源对金属材料加热气化，以在转移涂层表面沉积生成金属薄膜可以更好的实现台阶覆盖度和大深孔径的微细孔的孔底覆盖。
通过上面描述的独立金属薄膜制备过程除了操作简单，成本低，并且在金属薄膜沉积和剥离过程中温度保持在室温水平，金属薄膜的热应力小，能够保持金属薄膜较佳韧性，以在剥离和使用中不容易碎裂。且能有效剥离出厚度在几十到几百纳米的整片3D结构金属薄膜材料。而且通过上述过程可以形成面积较大的独立金属薄膜，独立金属薄膜的面积最大可达10cm*10cm。
另，本发明的金属薄膜，可以采用上面所述分方法进行制备。通过上面的独立金属薄膜制备方法可以制备最终需要的独立金属薄膜，还满足更多的使用场景。通过上述方法获得的金属薄膜热应力小，能够保持金属薄膜较佳的韧性，在使用中不容易碎裂。 
可以理解的，以上实施例仅表达了本发明的优选实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制；应当指出的是，对于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，可以对上述技术特点进行自由组合，还可以做出若干变形和改进，这些都属于本发明的保护范围；因此，凡跟本发明权利要求范围所做的等同变换与修饰，均应属于本发明权利要求的涵盖范围。

Claims (10)

  1. 一种独立金属薄膜制备方法，其特征在于，包括以下步骤：
    S1、旋涂转移涂层：选择表面满足光学级平整度的衬底，对所述衬底进行清洗烘干并在所述衬底表面上旋涂转移涂层；
    S2、固化：蒸发并冷却旋涂所述转移涂层后的衬底，以固化所述转移涂层；
    S3、沉积：选用金属材料，在固化的转移涂层表面沉积以生成预设厚度的金属薄膜；所述沉积包括：
    在真空条件下充入氩气，并通过溅射电源在所述转移涂层表面沉积生成所述金属薄膜；或
    在真空条件下通过电子束电源对所述金属材料加热气化，以在所述转移涂层表面沉积生成所述金属薄膜；
    S4、剥离：在常温下将带有所述金属薄膜的衬底置于可溶解所述转移涂层的有机溶剂中，以分离所述金属薄膜；
    S5、转移：保持所述金属薄膜为展开状态并转移所述金属薄膜至无氧条件下烘干，以得到最终的独立金属薄膜。
  2. 根据权利要求1所述的独立金属薄膜制备方法，其特征在于，在所述步骤S1中，所述在所述衬底表面上旋涂转移涂层过程中，所述转移涂层厚度为所述金属薄膜的预设厚度的0.5-2倍。
  3. 根据权利要求1所述的独立金属薄膜制备方法，其特征在于，在所述步骤S3中，在所述在固化的转移涂层表面沉积以生成预设厚度的金属薄膜过程中，所述衬底温度不超过80℃。
  4. 根据权利要求2所述的独立金属薄膜制备方法，其特征在于，在所述步骤S3中，所述在真空条件下充入氩气包括：充入氩气至气压满足0.4-4Pa。
  5. 根据权利要求1所述的独立金属薄膜制备方法，其特征在于，在所述步骤S3中，所述金属薄膜的预设厚度为50-1000nm。
  6. 根据权利要求1所述的独立金属薄膜制备方法，其特征在于，在所述步骤S1中，所述衬底的表面平整度为±10nm/cm 2。
  7. 根据权利要求1所述的独立金属薄膜制备方法，其特征在于，在所述步骤S3中，所述金属材料为Au、Ag、Cu、Cr、Al、Ni、Ti中的一种或多种。
  8. 根据权利要求1所述的独立金属薄膜制备方法，其特征在于，在所述步骤S5中，所述转移过程包括，使用网状结构或中空的环形框工具对所述金属薄膜进行托举以保持所述金属薄膜为展开状态。
  9. 根据权利要求1所述的独立金属薄膜制备方法，其特征在于，在所述步骤S2后，还执行以下步骤：
    S2-1、预设图案：在固化后的转移涂层表面设置预设图案。
  10. 一种金属薄膜，其特征在于，通过权利要求1-9任意一项所述的独立金属薄膜制备方法制备获取。
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030159920A1 (en) * 1998-07-17 2003-08-28 Micro Therapeutics, Inc. Thin film stent
JP2008074671A (ja) * 2006-09-21 2008-04-03 Tohoku Univ 自立窒化物基板の製造方法
WO2009102009A1 (ja) * 2008-02-15 2009-08-20 National Institute Of Advanced Industrial Science And Technology 水素分離用フィルム状自立金属薄膜およびその製造方法
CN102627258A (zh) * 2012-04-23 2012-08-08 中国科学院高能物理研究所 亚微米级自支撑聚酰亚胺薄膜及其制备方法
CN103043600A (zh) * 2012-12-13 2013-04-17 中国科学院物理研究所 基于薄膜材料的三维自支撑微纳米功能结构的制备方法
CN106544629A (zh) * 2017-01-19 2017-03-29 中国工程物理研究院激光聚变研究中心 一种大尺度自支撑铍薄膜的制备方法及装置

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030159920A1 (en) * 1998-07-17 2003-08-28 Micro Therapeutics, Inc. Thin film stent
JP2008074671A (ja) * 2006-09-21 2008-04-03 Tohoku Univ 自立窒化物基板の製造方法
WO2009102009A1 (ja) * 2008-02-15 2009-08-20 National Institute Of Advanced Industrial Science And Technology 水素分離用フィルム状自立金属薄膜およびその製造方法
CN102627258A (zh) * 2012-04-23 2012-08-08 中国科学院高能物理研究所 亚微米级自支撑聚酰亚胺薄膜及其制备方法
CN103043600A (zh) * 2012-12-13 2013-04-17 中国科学院物理研究所 基于薄膜材料的三维自支撑微纳米功能结构的制备方法
CN106544629A (zh) * 2017-01-19 2017-03-29 中国工程物理研究院激光聚变研究中心 一种大尺度自支撑铍薄膜的制备方法及装置

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