WO2021057922A1 - 一种真空镀膜装置 - Google Patents

一种真空镀膜装置 Download PDF

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Publication number
WO2021057922A1
WO2021057922A1 PCT/CN2020/117883 CN2020117883W WO2021057922A1 WO 2021057922 A1 WO2021057922 A1 WO 2021057922A1 CN 2020117883 W CN2020117883 W CN 2020117883W WO 2021057922 A1 WO2021057922 A1 WO 2021057922A1
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WIPO (PCT)
Prior art keywords
sub
nozzle
outlet
crucible
vacuum coating
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PCT/CN2020/117883
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English (en)
French (fr)
Inventor
任三兵
樊俊飞
李山青
熊斐
汪义如
Original Assignee
宝山钢铁股份有限公司
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Application filed by 宝山钢铁股份有限公司 filed Critical 宝山钢铁股份有限公司
Priority to US17/762,302 priority Critical patent/US20220356556A1/en
Priority to EP20868378.9A priority patent/EP4012067B1/en
Priority to JP2022519381A priority patent/JP7407916B2/ja
Priority to KR1020227008548A priority patent/KR20220046657A/ko
Publication of WO2021057922A1 publication Critical patent/WO2021057922A1/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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
    • 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
    • C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
    • 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
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of 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
    • 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
    • C23C14/243—Crucibles for source material
    • 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
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • C23C14/543—Controlling the film thickness or evaporation rate using measurement on the vapor source

Definitions

  • the invention relates to the technical field of vacuum coating, and more specifically, to a vacuum coating device.
  • PVD Physical vapor deposition
  • electric heating resistance or induction
  • EBPVD electron beam gun heating
  • the key issue in the vacuum coating process is how to obtain a uniform coating with consistent thickness through the arrangement of nozzles.
  • the information disclosed abroad mainly includes the following aspects:
  • Patent applications BE1009321A6 and BE1009317A61 respectively disclose the crucible nozzle structure as shown in Figure 1 and Figure 2.
  • a cover 2 is added to the upper part of the crucible 1, so that a nozzle structure is formed between the upper cover 2 and the furnace wall for direct injection of evaporated metal.
  • the filter plate 3 is added to the evaporation crucible, and then the metal vapor is sprayed from the slit nozzle on the top.
  • the nozzle design process of these two devices one adopts the Laval nozzle structure, and the other adopts the shrinking nozzle, and the orientation of the nozzle is one side jet and the other vertical jet.
  • Figure 3 shows a crucible nozzle structure with automatic liquid metal replenishment.
  • the nozzle 4 uses a wider outlet, and a heater 5 is also arranged on the upper part of the crucible for heating.
  • the structure is expanded by an arc 6 on one side, spraying sideways, and a heating tube 7 is also arranged on the outside of the crucible wall for wall heating.
  • Patent application WO2018/020311A1 discloses a split crucible nozzle structure, as shown in Figure 5, in this device, the bottom of the crucible is connected to a molten metal supply tank 8, and the upper part of the supply tank 8 passes the split pipe 9 to the metal vapor It is sent to the tubular distributor and the steam nozzle at the front end, and then the nozzle sprays the metal steam to the metal sheet at a high speed.
  • Patent application CN103249860A discloses a split flow distributor and nozzle structure. As shown in Figure 6, steam is sent to the upper horizontal pipe 10 through a vertical pipe. The top of the horizontal pipe 10 is provided with a porous nozzle to remove metal steam. Spray evenly on the surface of the sheet metal.
  • Patent application CN101175866A discloses a metal vapor distributor and nozzle form.
  • the cross-sectional form of the nozzle is shown in Fig. 7.
  • the distributor pipe 11 is wound with a wire to heat the pipe.
  • the nozzle has a square shell, as shown in Fig. 8.
  • a ring-shaped pipe made of another material is nested inside the square shell 12 for the injection of metal steam, and the steam outlet used by the nozzle is a porous type.
  • the purpose of the present invention is to provide a vacuum coating device that can form a uniform jet, so that when the high-temperature steam contacts the low-temperature steel plate, a uniform coating can be formed on the surface of the steel plate, and subsequent sub-nozzles are formed.
  • the jet stream continuously covers the vapor-deposited metal layer that has been formed, so as to achieve high-efficiency coating of the steel strip under vacuum conditions.
  • a vacuum coating device which is located below the steel plate when in use, includes a crucible, an induction heater is arranged on the outside of the crucible, and the top of the crucible is connected with a flow box through a steam pipe, in the steam pipe A pressure regulating valve and a diverting valve are provided, and the diverting valve is closer to the distribution box than the pressure regulating valve.
  • the distribution box is provided with a horizontal stabilizing plate, and the top of the distribution box is connected with several sub nozzle;
  • the diverter valve equipped with a plurality of air distribution chambers, the air distribution chamber radially than the total sectional area S of the bypass duct radially to the steam pipe cross sectional area S of 0.1, namely:
  • the ratio of S split to S pipe is less than 0.1, the flow rate of steam injection is too small to meet the thickness requirements of the coating; if the ratio of S split to S pipe exceeds 1, the flow velocity at the outlet of the sub-nozzle will be reduced, resulting in coating and The adhesion of the steel plate is reduced. Therefore, further, the S split /S pipe is 0.1-1.
  • the sub-nozzles are arranged in parallel and equidistant, the sub-nozzles have sub-nozzle outlets, and the relationship between the distance between the sub-nozzle outlets and the running speed of the steel plate is as follows:
  • the centerline distance of the outlet of the sub-nozzle is 100-150mm
  • the distance of the center line of the outlet of the sub-nozzle is 200-300 mm.
  • the shorter spray distance is used.
  • the spray cone formed after the steam is sprayed from the nozzle outlet has a shorter length covering the steel plate, the thickness of the spray can still meet the corresponding requirements; however, when the steel plate moves at a speed When speeding up, if you want to achieve the same coating thickness, you can adjust the distance between the sub-nozzle and the steel plate. As the distance increases, the length of the spray cone covering the steel plate increases. At this time, the steel plate enters the spray cone from the start point to when it leaves. The end time of the spray cone is increased, and the spray layer formed by the subsequent sub-nozzles continuously covers the previously formed plating layer, and the thickness of the plating film after superposition can meet the requirements.
  • the outlet of the sub-nozzle is set to be a slit type or a porous type, and the sum of the area of the outlet of the sub-nozzle S is the area of the connection position between the outlet and the steam pipe and the top of the crucible S inlet (or the crucible and the steam pipe
  • the ratio of the area of the junction (S entrance ) is 0.05-5. If the ratio is less than 0.05, the flow rate of the steam injection is too small to meet the thickness requirements of the coating. If the ratio is too large, such as greater than 5, the steam velocity at the nozzle outlet will be very small, resulting in a decrease in the adhesion of the coating .
  • the outlet of the slit-type sub-nozzle is arranged in a linear shape or a curved shape.
  • the outlet of the porous sub-nozzle is arranged in a rectangular, circular or trapezoidal shape, or in other words, is arranged in an arbitrary polygonal or circular shape.
  • the sub-nozzle is made of high-temperature-resistant and wear-resistant materials, and the above-mentioned processing can be performed on the structure.
  • it is made of graphite, ceramic or inert metal materials.
  • the shape of the hole on the voltage stabilizing plate is rectangular, circular or triangular, or the shape of the hole can be any polygonal or circular shape.
  • the direction of the pores of the stabilizing plate is a straight line, a curve or a multilayer structure along the rising direction of the steam. Since the pressure stabilizing plate has a certain thickness, the direction of the pores refers to the path of steam passing through the thickness direction of the stabilizing plate. The distribution can be changed, and the rising path of the vapor can also be changed by the pore direction.
  • the multi-layer structure refers to a structure in which the pores guide the steam to rise in steps, such as an airflow step formed by multiple sets of broken lines. This structure will increase the resistance of the stabilizing plate to the airflow, but can make the steam more evenly distributed.
  • the pressure-stabilizing plate can also be a porous medium pressure-stabilizing plate.
  • This type of pressure-stabilizing plate filters gas through irregular pores similar to honeycombs, and can adopt different porosity according to production needs. Change the airflow distribution, so as to achieve the purpose of uniform airflow.
  • S ratio of the area of the inlet of the regulator board total pore area S total pore area of the steam pipe and connected to the crucible top position is greater than or equal to 0.1, that is: the total pore area S / S inlet ⁇ 0.1.
  • the pressure and velocity of the outlet of the sub-nozzle can be adjusted.
  • the ratio is less than 0.1, the velocity of the gas passing through the outlet of the sub-nozzle will be too low, thereby reducing the adhesion of the coating.
  • the ratio is greater than 10 energy dissipation will occur, resulting in that the velocity of the airflow at the outlet of the sub-nozzle cannot be significantly increased.
  • the metal vapor is obtained by melting and evaporating the metal by heating the metal in an induction crucible.
  • the steam enters the distribution box through a pipe, and the distribution box is equipped with a diverter valve and a stabilizing plate. After the metal vapor passes through the diverter valve The flow direction changes and is divided into 2 to 5 steam streams. These steam streams are then distributed to the corresponding sub-nozzles.
  • the distribution box has a porous structure stabilizing plate near the inner sub-nozzles, and the sub-nozzles are arranged in parallel and equidistant. When the steam passes through the stabilizing plate, it is sprayed from the sub-nozzles at various levels to form a uniform jet.
  • Figure 1 is a schematic diagram of the patent application BE1009321A6;
  • Figure 2 is a schematic diagram of the patent application BE1009317A61
  • FIG. 3 is a schematic diagram of the patent application JPS59177370A
  • Figure 4 is a schematic diagram of the patent application US4552092A
  • Figure 5 is a schematic diagram of patent application WO2018/020311A1;
  • Figure 6 is a schematic diagram of patent application CN103249860A
  • Figure 7 is a schematic diagram of patent application CN101175866A
  • Fig. 8 is a schematic diagram of the square housing in Fig. 7;
  • Figure 9 is a schematic diagram of the structure of the vacuum coating device of the present invention.
  • Figure 10 is a schematic diagram of the internal type of the diverter valve in the vacuum coating device of Figure 9, in which (a) is a three-stage diverter valve, (b) is a four-stage diverter valve, and (c) is a two-stage diverter valve.
  • Fig. 11 is a schematic diagram of S branch and S pipeline in the shunt valve of Fig. 10;
  • Fig. 12 is a schematic diagram of the total area of S pores, S inlet and S outlet positions in the vacuum coating device of the present invention.
  • a vacuum coating device provided by the present invention, the vacuum coating device is located under the steel plate 100 during operation, the vacuum coating device includes a crucible 13, the crucible 13 is filled with molten metal 14.
  • An induction heater 15 is provided on the outside of the crucible 13, and the top of the crucible 13 is connected to a flow box 17 through a steam pipe 16, and the steam pipe 16 is sequentially provided with a pressure regulator in the direction leading to the flow box 17
  • the valve 18 and the diverter valve 19 are provided with a horizontal stabilizing plate 20 in the flow distribution box 17, and a number of sub-nozzles 21 are connected to the top of the flow distribution box 17.
  • the shape of the diverter valve 19 can be various shapes such as circle, triangle, trapezoid, rectangle, etc. Its main function is to evenly distribute the steam passing through the pipe to the corresponding sub-nozzles in the steam pipe 16.
  • the diverter valve 19 equipped with a plurality of air distribution chambers 1901, the radial cross-sectional area than the radial air-distribution chamber 1901 of the total sectional area S of the bypass duct 16 of the steam pipe S is greater than or equal to 0.1, i.e., : S shunt /S pipeline ⁇ 0.1. Further, the S split /S pipe is 0.1-1.
  • n-level sub-nozzle in this application refers to the number of working nozzles.
  • the 2-level sub-nozzle refers to two sub-nozzles working
  • the 3-level sub-nozzle refers to three sub-nozzles working, and so on.
  • n is equal to the number of distribution chambers 1901.
  • n is an integer of 2-5.
  • the sub-nozzles are arranged linearly and equidistantly along the moving direction of the steel plate, the sub-nozzles have sub-nozzle outlets, and the distance between the center lines of the sub-nozzle outlets and the operating speed of the steel plate 100 are related as follows:
  • the centerline distance of the outlet of the sub-nozzle is 50-100mm
  • the centerline distance of the outlet of the sub-nozzle is 100-150mm;
  • the centerline distance of the outlet of the sub-nozzle is 200-300 mm.
  • the internal pressure of the sub-nozzle during operation is 500-500,000 Pa.
  • the material of the sub-nozzle 21 can be graphite, ceramic or inert metal, and other materials that can be processed.
  • the sub-set to nozzle outlet slit type or a porous type, and the nozzle outlet area S of the sub-outlet 16 to the steam pipe and said inlet of the crucible area ratio S is connected to the top position 13 0.05 ⁇ 5.
  • the outlet of the sub-nozzle adopts a slit type, and the outlet of the slit-type sub-nozzle is arranged in a linear shape or a curved shape.
  • the voltage stabilizing plate 20 is arranged in a porous structure of any shape, and the pores of the voltage stabilizing plate 20 have a straight line, a curve, or a multilayer structure.
  • the inlet of the regulator plate area ratio S total pore area S total pore area on the steam pipes 16 and 20 and the position of the crucible 13 is connected to the top of 0.1 or greater, and less than or equal to 10, i.e., :0.1 ⁇ S total area of pores /S entrance ⁇ 10
  • the molten metal 14 may contain metals such as zinc, magnesium, aluminum, tin, nickel, copper, and iron, in addition to low melting point (less than 2000° C.) oxides of these elements.
  • the steel plate 100 is cleaned by a plasma device before vacuum coating, and the preheating temperature reaches 80-300°C.
  • the specific working process of the vacuum coating device of the present invention is as follows:
  • the metal block is heated by the induction heater 15 in the crucible 13 to melt into the molten metal 14.
  • the molten metal 14 starts to vaporize under higher superheat and low pressure, and gradually forms the metal vapor 22;
  • the metal steam 22 flows along the steam pipe 16 to the distribution box 17.
  • the diverter valve 19 divides the steam flow into 2 to 5 streams, and these steam streams are then distributed to the corresponding distribution box In 17, there is a pressure stabilizing plate 20 with a porous structure inside the flow distribution box 17, and the sub-nozzles 21 are arranged in parallel and equidistant between them;
  • the steam stream reduces the pressure of the dispersed high-speed flow, and flows out evenly along the small holes on the stabilizing plate 20, and then uniformly flows out from the outlet of the sub-nozzle 21, due to the sub-nozzle 21
  • the outlet is narrow, which makes the metal vapor 22 flow out at a higher speed
  • a moving steel plate 100 is arranged above it, and the temperature of the metal vapor 22 is relatively high. When it encounters the steel plate 100 with a lower temperature, it solidifies rapidly, forming a metal coating 23. Since the sub-nozzles are arranged equidistantly along the direction of steel plate movement, a large thickness of coating can be completed at one time.
  • the surface of the steel sheet 100 is galvanized, and the width of the steel sheet 100 is 1000 mm. After washing and drying, the steel sheet 100 is heated to 150°C.
  • the induction heater 15 heats the zinc to evaporate, and controls the power so that the pressure in the crucible 13 reaches 30000 Pa, and the pressure regulating valve 18 is closed before this.

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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)
  • Physical Vapour Deposition (AREA)

Abstract

提供一种真空镀膜装置，包括坩埚（13），坩埚（13）外侧设有感应加热器（15），坩埚（13）顶部通过蒸汽管道（16）连有布流箱体，蒸汽管道（16）通向布流箱体方向上依次设有调压阀（18）和分流阀（19），布流箱体内设有一水平向的稳压板（20），布流箱体顶部连有若干个子喷嘴（21）；分流阀（19）内设有若干个气流分配腔，气流分配腔的总面积S 分流与蒸汽管道（16）的径向面积S 管道之比大于等于0.1，即：S 分流/S 管道≥0.1。该装置能形成均匀的喷射流，使高温蒸汽和低温钢板接触时，在钢板（100）表面形成均匀镀层（23），排列在后方的子喷嘴（21）形成的喷射流不断地覆盖在已经形成的蒸镀金属层上，从而实现在真空条件下对带钢的高效镀膜。

Description

一种真空镀膜装置 技术领域
本发明涉及真空镀膜技术领域，更具体地说，涉及一种真空镀膜装置。
背景技术
物理蒸发镀(PVD)是指在真空条件下加热被镀金属，使之以气态的方式沉积到基材上形成镀膜的工艺技术。根据加热方式的不同又分为电加热(电阻或感应式)和电子束枪加热(EBPVD)等。真空镀膜作为表面改性和镀膜工艺，已经在电子、玻璃、塑料等行业得到了广泛的应用，真空镀膜技术主要优点在于其环保、良好的镀膜性能和可镀物质的多样性。连续带钢运用真空镀膜技术的关键在于镀膜生产连续化、大面积、高速率、大规模等几个方面。从上世纪八十年代开始，世界各大钢铁公司都对此技术进行了大量的研究。随着热镀锌和电镀锌技术的成熟，该技术正在受到空前的重视，并被认为是创新型的表面镀膜工艺。
真空镀膜过程中的关键问题是如何通过喷嘴的布置得到厚度一致的均匀镀层。目前国外公开的资料中，主要包含以下几个方面：
1)蒸发坩埚与布流喷嘴一体式结构
专利申请BE1009321A6、BE1009317A61分别公开了如图1、图2的坩埚喷嘴结构。在图1的结构中，坩埚1上部加上盖2，使得上盖2和炉壁之间形成喷嘴结构，用于蒸发金属的直接喷射。在图2的结构中，则在蒸发坩埚中添加过滤板3，而后由顶部的狭缝喷嘴喷射金属蒸汽。在这两个装置的喷嘴设计过程中，一个采用了拉瓦尔喷嘴结构，另一个采用了收缩喷嘴，而喷嘴的朝向位置一个是侧向喷射，另一个是垂直喷射。
在专利申请JPS59177370A、US4552092A中亦公开了相关蒸发坩埚及喷嘴结构。图3给出了一种带自动补充金属液的坩埚喷嘴结构，喷嘴4采用较宽的出口，在坩埚上部也布置了加热器5用于加热。图4给出的坩埚喷嘴结构中其结构由一侧的弧形6展开，侧向喷射，在坩埚壁的外侧同样 布置了加热管7用于壁面的加热。
2)蒸发坩埚与布流喷嘴分体式结构
专利申请WO2018/020311A1公布了一种分体式坩埚喷嘴结构，如图5所示，在该装置中，坩埚的底部连接一个金属液供给槽8，供给槽8的上部通过分体式管道9将金属蒸汽送至管状的分配器和前端的蒸汽喷嘴中，而后，喷嘴将金属蒸汽高速喷射至金属板材。
专利申请CN103249860A公开了一种分体式布流器及喷嘴结构，如图6所示，通过一个竖直管道将蒸汽送至上部水平管道10中，水平管道10顶部具有多孔喷嘴，用以将金属蒸汽均匀地喷涂在金属板材表面。
专利申请CN101175866A公开了一种金属蒸汽布流器及喷嘴形式，如图7所示的喷嘴的截面形式，布流器管道11外部缠绕导线从而实现对管道的加热，喷嘴具有方形外壳，如图8所示，方形外壳12内部嵌套了另一种材质的环形管道，用于金属蒸汽的喷射，喷嘴使用的蒸汽出口形式为多孔式。
上述这些专利都涉及喷嘴的具体形式，但是并不能表明利用这些喷嘴进行的镀膜都足够均匀，例如图6和图7，由于喷嘴的小孔采用间隔的圆孔，高压气体沿小孔喷出以后会形成放射状的圆斑，在钢板运动的过程中，如果圆斑和圆斑之间不重合，则很容易形成长条状的涂层；如果圆斑和圆斑之间太靠近，则圆斑之间的重合部分又容易形成较厚的涂层，不重合部分形成较薄的涂层，从而导致钢板涂层不均匀。
此外，这些专利并未给出如何实现对带钢快速高效的真空镀膜方法。从现场带钢生产线的匹配来说，在高拉速的情况下，如果想使真空镀的镀锌流量一次达到要求，需要不断地增大输送管直径和增加蒸发器的容积，与此同时还需增大喷嘴的开口度，然而开口度的增大不利于纵向截面形成均匀的镀层，需要避免。
发明内容
针对现有技术中存在的上述缺陷，本发明的目的是提供一种真空镀膜装置，能形成均匀的喷射流，使高温蒸汽和低温钢板接触时，能在钢板表 面形成均匀镀层，后续子喷嘴形成的喷射流不断地覆盖在已形成的蒸镀金属层上，从而实现在真空条件下对钢带的高效镀膜。
为实现上述目的，本发明采用如下技术方案：
一种真空镀膜装置，所述真空镀膜装置在使用时位于钢板的下方，包括坩埚，坩埚外侧设有感应加热器，所述坩埚顶部通过蒸汽管道连有布流箱体，在所述蒸汽管道内设有调压阀和分流阀，并且分流阀比调压阀更靠近布流箱体，所述布流箱体内设有水平向的稳压板，所述布流箱体顶部连有若干个子喷嘴；
所述分流阀内设有若干个气流分配腔，所述气流分配腔径向的总截面积S 分流与所述蒸汽管道径向的截面积S 管道之比为0.1，即：
S 分流/S 管道≥0.1。
如果S 分流与S 管道的比值小于0.1，则蒸汽喷射的流量太小，无法满足镀膜的厚度要求；如果S 分流与S 管道的比值超过1，会使得子喷嘴出口的流速变小，导致镀膜与钢板的粘合力降低。因此，进一步地，S 分流/S 管道为0.1～1。
所述子喷嘴为平行等距设置，所述子喷嘴具有子喷嘴出口，所述子喷嘴出口间距与所述钢板运行速度关系如下：
当所述钢板运行速度为30～60m/min时，所述子喷嘴出口中心线距离为50～100mm；
当所述钢板运行速度为61～100m/min时，所述子喷嘴出口中心线距离为100～150mm；
当所述钢板运行速度为101～150m/min时，所述子喷嘴出口中心线距离为150～200mm；
当所述钢板运行速度为151～200m/min时，所述子喷嘴出口中心线距离为200～300mm。
当钢板运动速度较小时，采用较近的喷射距离，虽然蒸汽从喷嘴出口喷出后形成的喷射锥覆盖钢板的长度较短，但喷射的厚度仍可以达到相应的要求；然而，当钢板运动速度加快时，如果要达到相同的镀膜厚度，则可以通过调节子喷嘴和钢板之间的距离来实现，距离增加，喷射锥覆盖到钢板的长度增大，此时钢板从进入喷射锥的起点至离开喷射锥的终点时间 增加，由后续子喷嘴形成的喷射层不断地覆盖在之前形成的镀层上，叠加后的镀膜厚度能够达到要求。
所述子喷嘴出口设置为狭缝型或多孔型，且所述子喷嘴出口的面积之和S 出口与所述蒸汽管道和所述坩埚顶部的连接位置的面积S 入口(或者说坩埚与蒸汽管道的交界处的面积S 入口)之比为0.05～5。如果该比值小于0.05，则蒸汽喷射的流量太小，无法满足镀膜的厚度要求，如果该比值过大，例如大于5，那么蒸汽在喷嘴出口的速度将会很小，导致镀膜的粘附性降低。
所述狭缝型子喷嘴出口设置为直线形或者曲线形。
所述多孔型子喷嘴出口设置为矩形、圆形或梯形，或者说设置为任意多边形或圆形。
所述子喷嘴采用耐高温、耐磨的材料制成，并能在结构上进行上述加工即可。例如由石墨、陶瓷或者惰性金属材质制成。
所述稳压板上的孔形状为矩形、圆形或三角形，或者说孔隙形状可以为任何多边形和圆形。所述稳压板的孔隙走向沿蒸汽的上升方向为直线、曲线或者多层结构。由于稳压板具有一定的厚度，孔隙走向即指蒸汽穿过稳压板厚度方向的路径，也就是说，蒸汽穿过稳压板时，不仅蒸汽的分布可以通过孔隙在稳压板上的位置分布来改变，蒸气的上升的路径也可通过孔隙走向来改变。所述多层结构是指孔隙走向引导蒸汽呈阶梯上升的结构，例如由多组折线形成的气流台阶，该结构会增加稳压板对气流的阻力，但能够使蒸汽更均匀地分布。
在本申请的技术方案中，稳压板也可以采用多孔介质稳压板，该种类型的稳压板通过类似蜂窝状的不规则孔隙过滤气体，并可根据生产需要，采用不同的孔隙率来改变气流分布，从而达到使气流均匀的目的。
所述稳压板上的孔隙总面积S 孔隙总面积与所述蒸汽管道和所述坩埚顶部连接的位置的面积S 入口之比大于等于0.1，即：S 孔隙总面积/S 入口≥0.1。通过该面积的比值，可以调整子喷嘴出口的压力和速度。当该比值不足0.1时，会导致气体通过子喷嘴出口的速度过小，从而降低镀层的粘合力。当该比值大于10时，则会出现能量的耗散，导致气流在子喷嘴出口的速度得不到明显提高。
本发明所提供的真空镀膜装置，金属蒸汽是由感应坩埚加热金属熔化蒸发获得，蒸汽通过管道进入到布流箱体，布流箱体中布置分流阀和稳压板，金属蒸汽通过分流阀后流向改变，分为2～5股蒸汽流，这些蒸汽流随后分配至相应的子喷嘴中，布流箱体靠近内部子喷嘴的位置具有多孔结构的稳压板，子喷嘴之间平行等距布置，当蒸汽通过稳压板后由各级子喷嘴喷出，形成均匀的喷射流，当高温蒸汽喷射流和低温钢板接触时，在钢板表面形成了均匀镀层。随后，沿钢板运动方向排列在后方的子喷嘴喷出的喷射流在钢板上形成新的金属层，新的金属镀层不断的覆盖在由排列在前方的子喷嘴喷射的蒸镀金属层上，从而使钢带同一方向运行一次就能形成现有技术中需要多次蒸镀才能达到的镀层厚度，避免了现有技术中因多次镀膜导致各镀层之间界面结合不佳的问题。本发明投入少，操作简单，未来可以和真空镀膜技术成套输出。
附图说明
图1是专利申请BE1009321A6的示意图；
图2是专利申请BE1009317A61的示意图；
图3是专利申请JPS59177370A的示意图；
图4是专利申请US4552092A的示意图；
图5是专利申请WO2018/020311A1的示意图；
图6是专利申请CN103249860A的示意图；
图7是专利申请CN101175866A的示意图；
图8是图7中方形外壳的示意图；
图9是本发明真空镀膜装置的结构示意图；
图10是图9真空镀膜装置中分流阀的内型示意图，其中，(a)是3级分流阀，(b)是四级分流阀，(c)是二级分流阀。
图11是图10分流阀中S 分流与S 管道示意图；
图12是本发明真空镀膜装置中S 孔隙总面积、S 入口、S 出口位置的示意图。
具体实施方式
下面结合附图和实施例进一步说明本发明的技术方案。
请结合图9至图12所示，本发明所提供的一种真空镀膜装置，所述真空镀膜装置在工作时位于钢板100的下方，该真空镀膜装置包括坩埚13，坩埚13内盛有金属液14，坩埚13外侧设有感应加热器15，所述坩埚13顶部通过蒸汽管道16连有布流箱体17，所述蒸汽管道16通向所述布流箱体17方向上依次设有调压阀18和分流阀19，所述布流箱体17内设有一水平向的稳压板20，所述布流箱体17顶部连有若干个子喷嘴21。
较佳的，所述分流阀19的形状可以是圆形、三角形、梯形及长方形等各种形状，其主要作用就是在所述蒸汽管道16内将经过管道内的蒸汽平均分配至各子喷嘴对应的布流箱体。所述分流阀19内设有若干个气流分配腔1901，所述气流分配腔1901径向的总截面积S 分流与所述蒸汽管道16的径向的截面积S 管道之比大于等于0.1，即：S 分流/S 管道≥0.1。进一步地，S 分流/S 管道为0.1～1。
较佳的，当使用2级子喷嘴21时，可采用如图10的(c)中分流阀19，当使用3级子喷嘴21时，可采用如图10的(a)中分流阀19，当使用4级子喷嘴21时，可采用如图10的(b)中分流阀19。本申请中的n级子喷嘴是指工作喷嘴的数量，例如2级子喷嘴是指有两个子喷嘴工作，3级子喷嘴是指有三个子喷嘴工作，依此类推。同时，n与分配腔1901的数量相等。一般来说，n选取2～5的整数。
较佳的，所述各子喷嘴沿钢板移动的方向呈直线形等距排列，所述子喷嘴具有子喷嘴出口，所述子喷嘴出口的中心线的间距与所述钢板100运行速度关系如下：
当所述钢板100运行速度为30～60m/min时，所述子喷嘴出口中心线距离为50～100mm；
当所述钢板100运行速度为61～100m/min时，所述子喷嘴出口中心线距离为100～150mm；
当所述钢板100运行速度为101～150m/min时，所述子喷嘴出口中心线距离为150～200mm；
当所述钢板100运行速度为151～200m/min时，所述子喷嘴出口中心 线距离为200～300mm。
较佳的，所述子喷嘴工作时的内部压力为500～500000Pa。
较佳的，所述子喷嘴21的材质可以为石墨、陶瓷或者惰性金属，以及其它可以进行加工的材料。
较佳的，所述子喷嘴出口设置为狭缝型或多孔型，且所述子喷嘴出口的面积S 出口与所述蒸汽管道16和所述坩埚13顶部的连接位置的面积S 入口之比为0.05～5。
较佳的，所述子喷嘴出口采用狭缝型，所述狭缝型子喷嘴出口设置为直线形或者曲线形。
较佳的，所述稳压板20设置为任意形状的多孔结构，所述稳压板20的孔隙的走向为直线、曲线或者多层结构。
较佳的，所述稳压板20上的孔隙总面积S 孔隙总面积与所述蒸汽管道16和所述坩埚13顶部连接的位置的面积S 入口之比大于等于0.1，且小于等于10，即：0.1≤S 孔隙总面积/S 入口≤10
较佳的，所述金属液14可包含的范围为锌、镁、铝、锡、镍、铜、铁等金属，此外还包含这些元素的低熔点(低于2000℃)氧化物。
较佳的，钢板100在真空镀膜前先经过等离子装置清洗，预热温度达到80～300℃。
本发明真空镀膜装置具体工作过程如下：
1)金属块体在坩埚13中受到感应加热器15的加热熔化成金属液14，金属液14在更高的过热度和低压下开始汽化，逐步形成金属蒸汽22；
2)开始阶段，与坩埚13相连的蒸汽管道16上的调压阀18处于关闭状态，随着金属液14不断的汽化，坩埚13内腔的蒸汽压力不断增大，当坩埚13内腔达到一定压力时(例如，5000～500000Pa)，开启调压阀18，使其尽可能保持恒定的压力流出；
3)此时需同时增大感应加热器15的功率从而弥补因开启调压阀18开而减小的压力，调整感应加热器15的功率范围，使得坩埚13内腔的压力保持在恒定的范围；
4)调压阀18开启后，金属蒸汽22沿蒸汽管道16向布流箱体17流动， 分流阀19将蒸汽流分为2～5股，这些蒸汽流股随后分配至相应的布流箱体17中，布流箱体17内部具有多孔结构的稳压板20，子喷嘴21之间采用平行等距布置；
5)蒸汽流股由于稳压板20的作用，使得分散的高速流压力降低，并均匀地沿稳压板20上的小孔流出，随后从子喷嘴21的出口均匀地流出，由于子喷嘴21的出口狭小，使得金属蒸汽22流出时形成了较大的速度；
6)此时在其上方布置了运动的钢板100，金属蒸汽22温度较高，遇到温度较低的钢板100时，迅速凝固，形成了金属镀膜23。由于各子喷嘴之间沿钢板运动的方向等距设置，可一次性完成较大厚度的镀膜。
实施例
钢板100表面蒸镀锌，钢板100的宽度为1000mm，进行清洗干燥后，将钢板100加热至150℃。感应加热器15加热将锌蒸发，并通过控制功率使得坩埚13内的压力达到30000Pa，此前调压阀18处于关闭状态。当坩埚13内的气体压力达到30000Pa后，打开调压阀18，金属蒸汽22进入蒸汽管道16，分流阀19采用圆形2级分流，其中S 分流/S 管道＝0.4，稳压板20为多孔结构，S 孔隙总面积/S 入口＝4，子喷嘴21内部工作压力为10000Pa，子喷嘴21材质为石墨，子喷嘴21出口采用直线形狭缝，其中S 出口/S 入口＝1。
本技术领域中的普通技术人员应当认识到，以上的实施例仅是用来说明本发明，而并非用作为对本发明的限定，只要在本发明的实质精神范围内，对以上所述实施例的变化、变型都将落在本发明的权利要求书范围内。

Claims (9)

  1. 一种真空镀膜装置，其特征在于：包括坩埚，所述坩埚外侧设有感应加热器，所述坩埚顶部通过蒸汽管道连有布流箱体，所述蒸汽管道通向所述布流箱体方向上依次设有调压阀和分流阀，所述布流箱体内设有水平向的稳压板，所述布流箱体顶部连有若干个子喷嘴；
    所述分流阀内设有若干个气流分配腔，所述气流分配腔径向的总截面积S 分流与所述蒸汽管道径向的截面积S 管道之比大于等于0.1，即：
    S 分流/S 管道≥0.1。
  2. 如权利要求1所述的真空镀膜装置，其特征在于：所述子喷嘴为平行等距设置，所述子喷嘴具有子喷嘴出口，所述子喷嘴出口间距与所述钢板运行速度关系如下：
    当所述钢板运行速度为30～60m/min时，所述子喷嘴出口中心线距离为50～100mm；
    当所述钢板运行速度为61～100m/min时，所述子喷嘴出口中心线距离为100～150mm；
    当所述钢板运行速度为101～150m/min时，所述子喷嘴出口中心线距离为150～200mm；
    当所述钢板运行速度为151～200m/min时，所述子喷嘴出口中心线距离为200～300mm。
  3. 如权利要求1所述的真空镀膜装置，其特征在于：所述子喷嘴出口设置为狭缝型或多孔型，且所述子喷嘴出口的面积之和S 出口与所述蒸汽管道和所述坩埚顶部的连接位置的面积S 入口之比为0.05～5。
  4. 如权利要求3所述的真空镀膜装置，其特征在于：所述狭缝型子喷嘴出口设置为直线形或者曲线形。
  5. 如权利要求3所述的真空镀膜装置，其特征在于：所述多孔型子喷嘴出口设置为矩形、圆形或梯形。
  6. 如权利要求3所述的真空镀膜装置，其特征在于：所述子喷嘴为石墨、陶瓷或者金属材质制成。
  7. 如权利要求1所述的真空镀膜装置，其特征在于：所述稳压板为多孔结构，孔的形状为矩形、圆形、三角形、梯形或者是狭缝形。
  8. 如权利要求1所述的真空镀膜装置，其特征在于：所述稳压板上的孔隙总面积S 孔隙总面积与所述蒸汽管道和所述坩埚顶部连接的位置的面积S 入 口之比大于等于0.1，即：
    S 孔隙总面积/S 入口≥0.1。
  9. 如权利要求8所述的真空镀膜装置，其特征在于：所述稳压板上孔隙的走向为直线、曲线或者多层结构。
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