WO2020010522A1 - Procédé de préparation d'un film métallique indépendant et film métallique - Google Patents

Procédé de préparation d'un film métallique indépendant et film métallique 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
Authority
WO
WIPO (PCT)
Prior art keywords
thin film
metal thin
transfer coating
substrate
metal
Prior art date
Application number
PCT/CN2018/095163
Other languages
English (en)
Chinese (zh)
Inventor
龚国华
何江
Original Assignee
深圳通感微电子有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 深圳通感微电子有限公司 filed Critical 深圳通感微电子有限公司
Priority to PCT/CN2018/095163 priority Critical patent/WO2020010522A1/fr
Publication of WO2020010522A1 publication Critical patent/WO2020010522A1/fr

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Classifications

    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)

Abstract

L'invention concerne un procédé de préparation d'un film métallique indépendant et un film métallique, le procédé comprenant les étapes suivantes : S1. revêtement par centrifugation d'un revêtement de transfert : sélectionner un substrat dont la surface est conforme à la planéité du niveau optique, laver et sécher le substrat, et revêtir par centrifugation d'un revêtement de transfert la surface du substrat ; S2. solidification : évaporer et refroidir le substrat après revêtement par centrifugation du revêtement de transfert de manière à solidifier le revêtement de transfert ; S3. dépôt : sélectionner un matériau métallique, et le laisser se déposer sur la surface du revêtement de transfert solidifié de manière à produire un film métallique d'une épaisseur prédéfinie ; S4. pelage : mettre le substrat qui porte le film métallique dans un solvant organique capable de dissoudre le revêtement de transfert à une température normale de façon à séparer le film métallique ; et S5. transfert : maintenir le film métallique dans un état déplié, transférer le film métallique en condition anaérobie et le sécher de façon à obtenir un film métallique indépendant final. La présente solution technique peut être utilisée pour préparer un film métallique indépendant qui répond aux exigences ; le procédé est simple et facile à mettre en œuvre, et le coût est faible.
PCT/CN2018/095163 2018-07-10 2018-07-10 Procédé de préparation d'un film métallique indépendant et film métallique WO2020010522A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/CN2018/095163 WO2020010522A1 (fr) 2018-07-10 2018-07-10 Procédé de préparation d'un film métallique indépendant et film métallique

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/CN2018/095163 WO2020010522A1 (fr) 2018-07-10 2018-07-10 Procédé de préparation d'un film métallique indépendant et film métallique

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WO2020010522A1 true WO2020010522A1 (fr) 2020-01-16

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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 (fr) * 2008-02-15 2009-08-20 National Institute Of Advanced Industrial Science And Technology Film métallique autoportant mince et léger pour la séparation de l'hydrogène et son procédé de production
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 (fr) * 2008-02-15 2009-08-20 National Institute Of Advanced Industrial Science And Technology Film métallique autoportant mince et léger pour la séparation de l'hydrogène et son procédé de production
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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