CN108977791B - A ohmic heating device for coiling deposit film under high temperature - Google Patents

A ohmic heating device for coiling deposit film under high temperature Download PDF

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CN108977791B
CN108977791B CN201810817978.5A CN201810817978A CN108977791B CN 108977791 B CN108977791 B CN 108977791B CN 201810817978 A CN201810817978 A CN 201810817978A CN 108977791 B CN108977791 B CN 108977791B
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base band
electrode
metal base
winding
wheel disc
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CN108977791A (en
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陶伯万
赵睿鹏
苟继涛
徐一鲡
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54Controlling or regulating the coating process
    • C23C14/541Heating or cooling of the substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates

Abstract

The invention relates to the field of film deposition preparation at high temperature, in particular to an electrified heating device for winding a deposited film at high temperature. The invention redesigns the electrode wheel disc group; the metal base band is arranged on the insulating roller of the electrode wheel disc, penetrates through the electrode rods of each pair and is in good contact with the electrode rods of each pair; the metal base band is prevented from deforming under the condition of clamping and stressing by the electrode bar due to the supporting action of the insulating roller on the metal base band, and the later application of a product is ensured; the bearing ensures that relative friction does not exist between the metal base band and the insulating roller so as to avoid damaging the surface of the metal base band; the insulating roller is directly attached to and contacted with the metal base band and rolls along with the movement of the metal base band, and the continuous winding process is completed. The invention is suitable for heating various metal substrates, has high heating rate, uniform temperature distribution and high energy efficiency, and can realize the continuous winding preparation of the multilayer film.

Description

A ohmic heating device for coiling deposit film under high temperature
Technical Field
The invention relates to the field of film deposition preparation at high temperature, in particular to the winding preparation of films on metal base bands with different widths or metal substrates with buffer layers on two sides, which can be used for various film preparation processes such as evaporation, sputtering, pulsed laser deposition, metal organic chemical vapor deposition and the like. In particular to an electric heating device for winding a deposition film at high temperature.
Background
In the field of thin film preparation, no matter what process technology is adopted, in order to realize the controllable growth of the thin film and achieve the purpose of regulating and controlling the components, the structure and the performance of the thin film, the substrate for thin film deposition is generally required to be heated. In order to simplify the construction of the device, the corresponding heating device should also be optimized and modified as necessary. Because the requirement of the film growth on the substrate temperature is strict, the development of the film deposition heating device with the characteristics of high temperature rise and drop speed, uniform and stable heating, good reliability and repeatability and the like is particularly important.
At present, the heating modes adopted for preparing the film mainly comprise resistance wire heating, electromagnetic induction heating and light heating.
The resistance wire heating is to transfer the generated heat to the substrate to be heated by introducing large current into the heating wire with larger resistance, so that the substrate reaches the required temperature. The temperature of the substrate can be controlled by adjusting the current passing through the heating wire, and the design of different heaters can greatly influence the current passing through. The mode of heating by adopting the resistance wire has the advantages of simple principle and low requirement on the substrate. The defects of the method are mainly high energy consumption, difficult maintenance, complex design and slow temperature rise and fall speed.
Electromagnetic induction heating, or simply induction heating, is one method of heating conductor materials. The heating device utilizes the electromagnetic induction principle to enable the interior of a heated material to generate current, and achieves the purpose of heating through the energy generated by eddy current. Induction heating has many advantages over traditional heating methods: high heating temperature, high heating speed, high heating efficiency, relatively low energy consumption and the like. The disadvantages are that the substrate directly heated by the method is required to be a conductive material, the shape is regular, the resistivity distribution is uniform, the skin effect is generated, and the adopted high-frequency alternating electromagnetic field can influence the surrounding equipment, and is not suitable for heating the thinner metal base band.
The optical heating is to heat the substrate material by using light beams generated by the lamp tube to penetrate through the high-temperature resistant glass. This has the advantage that the substrate can be heated to the required temperature quickly and with a high thermal efficiency. However, as the thin film is deposited, the heating temperature on the transparent glass is unstable due to the adhesion of the thin film material, which affects the quality of the prepared thin film.
For a long strip-shaped metal substrate, the shape of a heater and the distribution of heating wires need to be well designed by adopting resistance wire heating to ensure that the temperature distribution along the length direction and the width direction of a metal strip is uniform, and the whole development process is relatively complex. The use of induction heating of a metal strip substrate requires a high frequency to reduce power consumption. Under high frequency, the plasma is easily generated in the vacuum cavity by the coupling excitation of a high-frequency electric field, which is not beneficial to the accurate control of the temperature.
In another mode of self-heating by energization, heating current is gradually introduced into the metal strip through a current distribution circuit, and joule heat generated by the resistance of the metal strip is utilized to achieve the purpose of heating. There is a related patent (CN201610881886.4) that uses a similar approach to heating a metal substrate. However, when the heating electrode in such a method heats a metal base band with a large width and a small thickness, the base band is deformed or distorted due to the action of pressure between the heating electrode elastic sheet and the base band, so that the electrode and the base band are in poor contact and ignition is caused, and the long strip material cannot be used in a later period, and continuous preparation of the long strip material is affected.
Disclosure of Invention
To above-mentioned problem or not enough that exists, when solving circular telegram self-heating metal baseband preparation film, the great and thin metal baseband of thickness of width can take place deformation or distortion to arouse electrode and baseband contact failure and strike sparks, thereby the unable problem of using in later stage. The invention provides an electric heating device for winding a deposited film at high temperature.
The electric heating device for winding the deposited film at high temperature is composed of a positive and negative electrode wheel disc, a film deposition area, an external power supply and two winding discs, wherein the positive and negative electrode wheel disc, the film deposition area, the external power supply and the two winding discs are installed in a vacuum cavity. The metal base band is drawn to an electrode wheel disc from a winding disc, is drawn to another electrode wheel disc after being coated with films in a film deposition area, and is finally collected by another winding disc, and an external power supply provides heating current for the electrode wheel disc.
The electrode wheel disc comprises an electrode group, a fixed disc, an insulating roller and a bearing. The principle of the heating mode is as follows: heating current is gradually led into the metal base band from the edges of the two sides of the base band through the electrode group and flows on the metal base band in the thin film deposition area, joule heat generated by the resistance of the base band reaches the temperature required by the growth of a thin film, and simultaneously flows out through another electrode group with the same structure to form a complete current path.
The electrode group consists of a metal elastic sheet, an electrode rod (such as an Ag-W alloy electrode rod) and a shunt resistor.
The fixed disc is used for mounting the whole electrode group, the bearing and the insulating roller and is made of insulating materials. The bearing is used for meeting the requirement of the metal base band for winding and coating, and the metal base band and the insulating roller have no relative friction so as to avoid damaging the surface of the metal base band. The insulating roller is directly attached to and contacted with the metal base band and rolls along with the movement of the metal base band, and the continuous winding process is completed.
The electrode group is composed of metal elastic sheets which are arranged on the same side at equal intervals and are symmetrically arranged on two sides of the fixed disk; the upper end of the electrode is fixed with electrode bars, each pair of electrode bars are electrically connected with each other and are connected with an external circuit. The metal base band is arranged on the insulating roller and penetrates through the electrode rods of each pair; the width of the metal base band is adapted to the width of the roller and is in good contact with each pair of electrode bars, and the edges of the two sides of the metal base band are in good contact with the electrode bars due to mutual pressure action.
The electrode rod adopts Ag-W alloy as an electrode material because the electrode rod has the characteristics of high conductivity and high melting point, has strong oxidation resistance, has the function of inhibiting electric arcs, and greatly reduces the occurrence of discharge and ignition phenomena between a base band and the electrode.
Because the metal base band and each pair of electrode rods slide relatively, the key of the metal base band electrifying heating mode is how to ensure that the base band and the electrodes still have good electric contact in the relative sliding state, and then the strong action between the metal elastic sheet and the edge of the base band is needed. However, when the metal base band is wider and thinner, the force between the metal elastic sheet and the two side edges of the base band will cause the base band to distort and deform, thereby causing poor contact and causing the phenomena of sparking and edge burning. Therefore, the metal elastic sheet provided with the electrode bar is integrated on the roller, the base band can be well supported, good electric contact with the electrode bar is guaranteed, deformation is avoided, the base band is always perpendicular to the electrode bar in the moving process, and reliability and stability of the broadband winding coating are improved.
The invention redesigns the electrode wheel disc group; the metal base band is arranged on the insulating roller of the electrode wheel disc, penetrates through the electrode rods of each pair and is in good contact with the electrode rods of each pair; the metal base band is prevented from deforming under the condition of clamping and stressing by the electrode bar due to the supporting action of the insulating roller on the metal base band, and the later application of a product is ensured; the bearing ensures that relative friction does not exist between the metal base band and the insulating roller so as to avoid damaging the surface of the metal base band; the insulating roller is directly attached to and contacted with the metal base band and rolls along with the movement of the metal base band, and the continuous winding process is completed. The invention is suitable for heating various metal substrates, has high heating rate, uniform temperature distribution and high energy efficiency, and can realize the continuous winding preparation of the multilayer film.
In summary, the present invention is suitable for heating metal base tapes of different widths and thicknesses or metal substrates having buffer layers (conductive or insulating) on both sides. And the heating rate is high, the temperature distribution is uniform, the energy efficiency is high, and meanwhile, the continuous winding preparation of the multilayer film can be realized. These advantages are especially important for the industrial preparation of the film, and can improve the quality of the prepared film and reduce the preparation cost of the film.
Drawings
Fig. 1 is a schematic perspective view of an electrode disk according to the present invention.
Figure 2 is a front view schematic of the electrode disk of the present invention.
Fig. 3 is an equivalent circuit diagram of the electrode wheel current distribution circuit.
FIG. 4 preparation of Gd on the example tape-shaped Metal base tape0.5Y0.5Ba2Cu3O7-x2Theta scan curve of XRD of (GdYBCO) film.
Fig. 5 is a plot of the ω -scan and the φ -scan of XRD for GdYBCO thin films on example strip metal substrates.
Reference numerals: 1-fixed disc, 2-bearing, 3-ceramic roller, 4-metal spring piece fixing bolt and nut, 5-metal spring piece, 6-electrode bar and 7-current distribution resistor.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
The electrode wheel disc shown in figure 1 is applied to the preparation of a GdYBCO high-temperature superconducting film.
The metal base band is drawn from one winding disc to one electrode wheel disc, passes through the film deposition area, is drawn to the other electrode wheel disc, is collected by the other winding disc, and is provided with heating current of the electrode wheel disc by an external power supply.
The insulating roller is made of ceramic, and the electrode bar is made of Ag-W alloy.
First, a Hastelloy alloy base tape (LaMnO) in which a buffer layer film has been prepared is prepared3/homo-epi MgO/IBAD-MgO/SDP-Y2O3Hastelloy) penetrates through the electrode wheel disc to realize good electric contact, the base band is connected to the two winding discs, an external power supply is connected, and a reaction chamber of the MOCVD system is vacuumized to be below 1 Pa.
Then, Gd (tmhd) was weighed3、Y(tmhd)3、Ba(tmhd)2And Cu (tmhd)2(thmd: 2, 2, 6, 6-tetramethyl-3, 5-heptanedione), and sufficiently dissolving the precursor in a tetrahydrofuran solvent to form a uniform and clear metal organic source precursor. And adjusting a current source, introducing heating current to the metal substrate, and drawing the metal substrate to the deposition area. Pumping the metal organic source precursor into an evaporation chamber at 300 ℃ by adopting a peristaltic pump to be flashed into metal organic source steam, and then reacting with O under the drive of Ar gas2And N2Mixing O gas, spraying the mixture to a metal base band by a spray head in a film deposition area after passing through a gas transmission pipeline at 320 ℃ to react to generate the GdYBCO film. The metal base strip after final deposition is collected by another winding disc via another electrode wheel disc.
Taking out a GdYBCO sample and placing the sample in a container with O2The tube furnace (2) was annealed at 500 ℃ for 30 minutes and finally the film was characterized. And (3) characterizing the structure of the prepared film:
FIG. 4 is a band-shaped metal substrate prepared with Gd0.5Y0.5Ba2Cu3O7-x2Theta scan curve of XRD of (GdYBCO) film. As can be seen from the figure, the diffraction peak intensity of the film (00l) surface is strong and sharp, and has no impurity peak, which shows that GdYBCO crystal grains grow along the pure c-axis direction and have good crystallization quality.
Fig. 5 is a plot of the ω -scan and the φ -scan of XRD for GdYBCO thin films on example strip metal substrates. From curve fitting in the figure, the values of the half-height width outside and inside the film are respectively 1.6 degrees and 2.9 degrees, which shows that the film has good orientation outside and inside the film.
In conclusion, the GdYBCO thin film prepared by the heating device has good crystallization quality and good out-of-plane in-plane orientation. The base band electrifying heating mode effectively overcomes the defects of the original heating system, has the advantages of simple principle and structure, high temperature rise and fall speed, high energy efficiency and easy expansion, can be suitable for heating metal base bands with different widths and thicknesses, improves the reliability, and can realize the continuous and stable winding preparation of single-sided or double-sided YBCO long strips.

Claims (2)

1. An electrical heating apparatus for winding a deposition film at a high temperature, characterized in that:
the device comprises a positive and negative electrode wheel disc, a film deposition area, an external power supply and two winding discs, wherein the positive and negative electrode wheel disc is arranged in a vacuum cavity; the metal base band is drawn to an electrode wheel disc from a winding disc, is drawn to another electrode wheel disc after being coated with a film in a film deposition area, and is finally collected by another winding disc, and an external power supply provides heating current for the electrode wheel disc;
the electrode wheel disc consists of an electrode group, a fixed disc, an insulating roller and a bearing; heating current is gradually led into the metal base band from the edges of the two sides of the base band through the electrode group and flows on the metal base band in the thin film deposition area, joule heat generated by the resistance of the base band reaches the temperature required by the growth of a thin film, and simultaneously flows out through another electrode group with the same structure to form a complete current path;
the electrode group consists of a metal elastic sheet, an electrode bar and a shunt resistor;
the fixed disc is used for mounting the whole electrode group, the bearing and the insulating roller and is made of insulating materials;
the bearing is used for meeting the requirement of the metal base band on winding and coating, and the metal base band and the insulating roller have no relative friction so as to avoid damaging the surface of the metal base band;
the insulating roller is directly attached to and contacted with the metal base band and rolls along with the movement of the metal base band to complete the continuous winding process;
the electrode group is composed of metal elastic sheets which are arranged on the same side at equal intervals and are symmetrically arranged on two sides of the fixed disk; electrode bars are fixed at the upper ends of the electrodes, and each pair of electrode bars are electrically connected with each other and are connected to an external circuit;
the metal base band is arranged on the insulating roller and penetrates through the electrode rods of each pair; the width of the metal base band is adapted to the width of the roller and is in good contact with each pair of electrode bars, and the edges of the two sides of the metal base band are in good contact with the electrode bars due to mutual pressure;
the electrode bar adopts Ag-W alloy as an electrode material.
2. An electric heating apparatus for winding a deposition film at a high temperature according to claim 1, wherein: the insulating roller is a ceramic roller.
CN201810817978.5A 2018-07-24 2018-07-24 A ohmic heating device for coiling deposit film under high temperature Active CN108977791B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100899355B1 (en) * 2007-11-15 2009-05-27 한국과학기술연구원 Plasma deposition apparatus and method
CN103276366B (en) * 2013-05-20 2015-07-22 上海超导科技股份有限公司 Box-type heater suitable for preparation process of roll-to-roll continuous strips
CN104046963B (en) * 2014-06-08 2016-08-24 电子科技大学 Thin film deposition preparation facilities and method
CN106521457A (en) * 2016-10-10 2017-03-22 电子科技大学 Heating device for high-temperature thin film deposition
CN206279263U (en) * 2016-12-30 2017-06-27 浙江尚越新能源开发有限公司 A kind of volume to volume magnetic-controlled sputtering coating equipment of substrate infrared heating
CN108220888B (en) * 2017-12-27 2019-12-27 上海超导科技股份有限公司 Heating device suitable for pulse laser coating and pulse laser coating device thereof

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