CN109097756B - Heating device for high-temperature thin film deposition of thin metal - Google Patents
Heating device for high-temperature thin film deposition of thin metal Download PDFInfo
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- CN109097756B CN109097756B CN201810995176.3A CN201810995176A CN109097756B CN 109097756 B CN109097756 B CN 109097756B CN 201810995176 A CN201810995176 A CN 201810995176A CN 109097756 B CN109097756 B CN 109097756B
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
Abstract
The invention belongs to the technical field of film preparation, and particularly relates to a heating device for high-temperature film deposition of thin metal. The invention redesigns the electrode group unit; the metal base band passes through N specially set conductive metal rods, is supported by the N specially set conductive metal rods and is in good contact with the N specially set conductive metal rods, and the conductive metal rods do not roll along with the movement of the metal base band. The conductive metal rod is in linear contact with the metal base band for conducting electricity, and the metal base band is supported so as not to deform, the ignition phenomenon is avoided, and the later application of the film is ensured. The invention is suitable for heating single-sided metal base bands with different widths and thicknesses; and the heating rate is high, the temperature distribution is uniform, the energy efficiency is high, and meanwhile, the continuous preparation of the multilayer film can be realized. These advantages are especially important for the industrial preparation of thin films, and can improve the quality of the prepared thin films and reduce the cost.
Description
Technical Field
The invention belongs to the technical field of film preparation, and particularly relates to a heating device for high-temperature film deposition of thin metal.
Background
In the field of thin film preparation, in order to control the growth of a thin film and further achieve the purpose of controlling the physicochemical properties of the thin film, it is generally necessary to heat a substrate to which the thin film is grown.
In the preparation of the film growth, an excellent reaction chamber is needed, the temperature of the reaction environment is required to be higher to match the design of the reaction chamber, and then a heater needs to be changed correspondingly. Because the gas reaction in the cavity has strict requirements on the temperature, a high-performance film deposition heating system with the characteristics of uniform temperature, rapid temperature rise and fall, stability, good repeatability and the like is required to be developed. Namely: the temperature is rapidly raised to the growth temperature for growing each layer of film; the heater can be controlled to realize different set temperatures, and the requirement of growing a multilayer deposited film is met; has good repeatability, and ensures that the material grown each time has the same property.
The following heating methods are common at present: (1) the heat conduction type heating is usually realized by adopting resistance wires, namely resistance wires with higher resistance are used, and large current is supplied, so that the resistance wires generate a large amount of joule heat in a short time, the temperature of the resistance wires is increased to 1500-2000 ℃, and then the heat is conducted to the substrate. The disadvantage is that the object to be heated is not too large to avoid poor contact between the substrate and the heating wire, which leads to non-uniform heating of the substrate. Moreover, the heating mode is not beneficial to the growth and preparation of the continuous strip film. (2) The radiation type heating is that the substrate is placed in the irradiation range of a high temperature heating body, and the substrate is heated by infrared rays radiated by the heating body, etc. Such a heating manner has strict requirements on the number, spatial distribution, etc. of the heating elements to ensure that the substrate obtains a sufficiently high and uniformly distributed temperature. However, in practical applications, such a heater design is difficult and requires a large amount of space. (3) Induction type heating, namely placing the conductor in a high-frequency electromagnetic field, inducing current with the passing frequency in the conductor, generating heat under the action of the current to heat and raise the temperature, wherein the heating rate of the heating mode is high, and the temperature of the surface of the substrate can reach 800-1000 ℃ within a few seconds. The heating method is not enough in that the substrate is heated, and the substrate is required to be an electric conductor with a certain thickness, and has a regular shape and uniform resistivity distribution. In addition, the heating method has high requirements on an induction power supply, and the device equipment is required to have good electromagnetic shielding so as to prevent surrounding electronic equipment and human bodies from being injured.
The heating modes have advantages and disadvantages, and the common point is that the energy required for heating the substrate is transferred or converted from the outside, but the energy actually required for heating the substrate is very little in the transferring or converting process, and most of the energy is wasted by the resistance wire or the power supply. When a thin film is formed on a wide, long, strip-shaped metal substrate, the heating method (1) is not suitable, particularly for a moving metal substrate. While the heating of (2) can be used for heating such a wide and long strip-shaped metal substrate, the heating source must be well designed to ensure uniform temperature distribution along the length and width of the metal substrate, but such a heating source is generally complicated. When the metal base band is heated by adopting the heating mode in the step (3), the skin depth limit value of the alternating electric field can be ensured to be in the material only by requiring very high electric field frequency so as to improve the energy efficiency. At high frequency, the coupling of the high frequency electric field is easily generated in the vacuum chamber to excite the plasma, so that the induction heating and the plasma occur simultaneously, which is disadvantageous to the precise control of the growth temperature.
When the strip-shaped metal substrate base band is heated, compared with the above-described conventional heating method, when the current is introduced into the metal substrate base band and the metal base band generates heat by its own resistance, the apparatus is simpler and more energy efficient. There is a related patent (CN106521457A) that uses a similar approach to heating a metal substrate. However, in this patent, two rows of electrode plates are adopted for placement, and the metal substrate base band is mostly a flexible strip, so that when a wide film is deposited, the metal substrate base band is bent inwards due to being too wide, and a discharge phenomenon caused by poor contact between the edge of the metal substrate base band and an electrode is caused, thereby being not beneficial to the film growth and preparation of the wide metal substrate base band.
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 a heating device for high-temperature thin film deposition of thin metals.
The heating device for high-temperature film deposition comprises a positive electrode group unit, a negative electrode group unit, a film growth area, an external current source and two winding disks, wherein the positive electrode group unit and the negative electrode group unit are arranged in a vacuum cavity. The metal base band (back conductive treatment) is drawn to one electrode group unit from one winding disc, is drawn to the other electrode group unit after being coated by the film growth area, and is finally wound on the other winding disc, and the external power supply provides heating current for the electrode group unit.
The electrode group unit consists of two rotating wheels, a conductive metal rod fixing device and a support frame and is used for heating the metal base band; the heating mode mechanism is as follows: heating current is led into the metal base band from the contact position of the base band and the metal base band through the conductive metal rod and flows on the metal base band in the film deposition area, joule heat generated by the resistance of the base band reaches the temperature required by film growth, and flows out through another electrode group with the same structure to form a complete current path.
The surface of the rotating wheel is smooth, no relative friction exists between the rotating wheel and the metal base band, the axis of the rotating wheel is insulated and is used for supporting the metal base band, one rotating wheel and the winding disc form a channel of the metal base band, and the other rotating wheel and the conductive metal rod and the film growth area form a channel of the metal base band respectively; the position of the metal base band is adjustable on the support frame so as to realize the contact force adjustment between the metal base band and the conductive metal rod.
The conductive metal bar is connected with an external power supply, supports and stabilizes the metal base band, and forms a channel of the metal base band with the rotating wheel; n conductive metal bars are fixed on the conductive metal bar fixing device in parallel at equal intervals, the end faces of the conductive metal bars on the same side are located on the same arc line on the conductive metal bar fixing device, the conductive metal bars and the conductive metal bar fixing device are insulated, and N is larger than or equal to 5. Each conductive metal rod and an external resistance unit form an electrode unit, the electrode units are electrically connected through a current distribution circuit, and the current distribution circuit is a series resistor. When the metal base band works, the metal base band is directly attached and contacted with the cambered surface formed by the N conductive metal rods, and the conductive metal rods do not roll along with the movement of the metal base band.
The support frame is used for installing the conductive metal bar fixing device and the two rotating wheels, and is insulated from the conductive metal bar fixing device and the rotating wheels.
Further, the current distribution circuit realizes the uniform distribution of current which is input to the metal base band through the conductive metal rod.
The invention redesigns the electrode group unit; the metal base strip is supported by and in good contact with N specially configured conductive metal bars. On one hand, the conductive metal rod is in linear contact with the metal base band to conduct electricity, so that a relatively uniform heating mode is formed; on the other hand, the metal base band cannot deform under the supporting action of the metal base band, so that the phenomenon of edge burning caused by poor contact is avoided, and the later-stage application of the product is ensured. The channel formed by the rotating wheel and the conductive metal rod enables the metal base band to be directly attached and contacted with the conductive metal rod, the conductive metal rod does not roll along with the movement of the metal base band, the good contact between the metal base band and the conductive metal rod is ensured, and the continuous winding process is completed through the two winding discs. The invention is suitable for heating various single-sided metal substrates, has high heating rate, uniform temperature distribution and high energy efficiency, and can realize continuous winding preparation of multilayer single-sided films.
In conclusion, the heating device is suitable for heating the single-sided metal base bands with different widths and thicknesses; 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 structural view of an apparatus according to an embodiment;
FIG. 2 is a schematic structural diagram of an electrode group unit according to an embodiment;
FIG. 3 is a partial top view of an embodiment electrode unit;
FIG. 4 is a schematic diagram of an embodiment current distribution circuit;
FIG. 5 is an x-ray diffraction 2Theta scan of a GdYBCO film at three different locations on a coated metal substrate of an example;
FIG. 6 is an x-ray diffraction Omega scan and Phi scan curve of a GdYBCO film at the middle position of a coated metal base band of an embodiment;
reference numerals: 1-winding disc 1, 2-rotating wheel, 3-support frame, 4-current distribution resistor, 5-conductive metal bar, 6-film growth area, 7-external current source, 8-conductive metal bar fixing device and 9-winding disc 2
Detailed Description
The invention is further described below with reference to the accompanying drawings and examples.
The device shown in figure 1 is used for the second generation high temperature superconducting tape Gd0.5Y0.5Ba2Cu3O7-xAnd (GdYBCO) film preparation. Taking a sectionA short sample 150mm long and 12mm wide was placed in the growth zone and had a buffer film deposited on the hastelloy flexible substrate (LaMnO)3/homo-epi MgO/IBAD-MgO/SDP-Y2O3Hastelloy), the back of the section of sample is polished to realize good electrical contact, then the section of sample is connected with a traction belt (a bare base belt) end to end in a welding mode, finally the positions of the metal substrate flexible base belt and a film growth area spray header are fixed and adjusted according to the embodiment, the traction belt is connected to a winding disc, and a circuit is connected. Weighing 128.5mg of Y (TMHD) of the metal organic source respectively3143.0mg of Gd (TMHD)3676.9mg of Ba (TMHD)3343.2mg of Cu (TMHD)3And 16.5mg of Zr (TMHD)3(TMHD:2,2,6, 6-tetramethyl-3, 5-heptanedione), dissolved together in 5ml of a tetrahydrofuran solvent, and placed in ultrasonic vibration to be sufficiently dissolved to form a uniform and clear metal organic source solvent. The power supply is turned on, and a current of 25.8A (voltage of about 39V) is applied to the flexible base band of the metal substrate. Opening a traction motor, and drawing the metal substrate flexible baseband sample to a film growth area; after the temperature is stable, namely the current power supply is not fluctuated, the metal organic source is sent into an evaporation chamber with the temperature of 310 ℃ for flash evaporation by adopting a peristaltic pump mode, and further metal organic source steam is formed; the metal organic source steam is further reacted with O under the drive of Ar2And N2And mixing O gas, spraying the O gas to a metal substrate flexible base band passing through a growth area through a gas transmission pipe at 320 ℃ through a spray head, and reacting to generate the GdYBCO film.
The conductive metal rod is an Ag-W alloy rod, the current for heating the metal substrate flexible baseband is high in the experimental process, namely the required temperature is high, the temperature of the metal substrate flexible baseband and the air pressure of a vacuum chamber are high, so that the electrode and the metal substrate flexible baseband are required to be in good electric connection, otherwise, the electrode and the baseband are burnt due to the discharge between the baseband and the electrode, and the Ag-W alloy rod has the characteristics of high conductivity and high melting point, is strong in oxidation resistance and has the function of printing electric arc, so that the Ag-W alloy rod is very suitable for the working environment.
The distribution current resistance diagram of the heating electrode is shown in fig. 4, and 6 Ag-W alloy rods are used in this embodiment, and assuming that the resistance of the Ag-W rods is negligible, in order to make the current on each Ag-W rod equal, the total current output by the current source is 6I assuming that the current is I. According to kirchhoff's law, the distribution resistance Rn is R × n/(6-n), and the distribution resistance in the embodiment is cut by using the same metal base band and calculating the structure according to the formula.
Placing the prepared GdYBCO sample into a container with O2The film sample was characterized after being taken out after 30 minutes of incubation at 500 ℃.
The structure of the prepared GdYBCO film is shown in figures 5 and 6.
In fig. 5, the diffraction peaks of (00l) planes at three different positions (two edges and middle) are all sharp, the intensities of the diffraction peaks are similar, and all the diffraction peaks have no impurity peak, which indicates that the GdYBCO crystal grains at the three positions are all pure c-axis growth, and also indicates that the crystal quality of the GdYBCO film on the metal substrate flexible baseband is uniform.
The out-of-plane and in-plane half-height-width values of the two curves in fig. 6 are 1.68 ° and 2.96 °, respectively, indicating that the GdYBCO film in this position has good out-of-plane and in-plane orientation and has a biaxial texture similar to that of the GdYBCO film on a single crystal.
Therefore, the GdYBCO film prepared by the heating device has good crystallization quality and orientation.
In summary, the heating mode of electrifying the base band from the back effectively overcomes the defects of the original heating system and the phenomenon that the base band is bent inwards due to the fact that current is led in from the edge of the base band due to the increase of the width of the flexible metal substrate; the heating mode can realize the continuous winding preparation of the GdYBCO film on the single surface of the wide and long metal substrate base band.
Claims (2)
1. A heating device for high-temperature thin film deposition of thin metal comprises a positive electrode group unit, a negative electrode group unit, a thin film growth zone, an external current source and two winding disks, wherein the positive electrode group unit, the negative electrode group unit, the thin film growth zone, the external current source and the two winding disks are arranged in a vacuum cavity, and the heating device is characterized in that:
the metal base band to be coated is drawn to an electrode group unit from a winding disc, is drawn to another electrode group unit after being coated by a film growth area, and is finally wound on another winding disc, and an external power supply provides heating current for the electrode group unit;
the electrode group unit consists of two rotating wheels, a conductive metal rod fixing device and a support frame and is used for heating the metal base band; the heating mode mechanism is as follows: heating current is led into the metal base band from the contact position of the base band and the metal base band through the conductive metal rod and flows on the metal base band in the film deposition area, and Joule heat generated by the resistance of the base band reaches the temperature required by film growth and flows out through another electrode group with the same structure to form a complete current path;
the surface of the rotating wheel is smooth, no relative friction exists between the rotating wheel and the metal base band, the axis of the rotating wheel is insulated and is used for supporting the metal base band, one rotating wheel and the winding disc form a channel of the metal base band, and the other rotating wheel and the conductive metal rod and the film growth area form a channel of the metal base band respectively; the position of the metal base band on the support frame is adjustable so as to realize the contact force adjustment between the metal base band and the conductive metal rod;
the conductive metal bar is connected with an external power supply, supports and stabilizes the metal base band, and forms a channel of the metal base band with the rotating wheel; n conductive metal bars are fixed on the conductive metal bar fixing device in parallel at equal intervals, the end faces of the conductive metal bars on the same side are positioned on the same arc line on the conductive metal bar fixing device, the conductive metal bars and the conductive metal bar fixing device are insulated, and N is more than or equal to 5; each conductive metal rod and an external resistance unit form an electrode unit, the electrode units are electrically connected through a current distribution circuit, and the current distribution circuit is a series resistor; when the metal base band works, the metal base band is directly attached and contacted with the cambered surface formed by the N conductive metal rods, and the conductive metal rods do not roll along with the movement of the metal base band;
the support frame is used for installing the conductive metal bar fixing device and the two rotating wheels, and the support frame is insulated from the conductive metal bar and the rotating wheels.
2. The heating apparatus for high temperature thin film deposition of thin metals as claimed in claim 1, wherein: the current distribution circuit realizes the uniform distribution of current and inputs the current to the metal base band through the conductive metal rod.
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| CN201810995176.3A CN109097756B (en) | 2018-08-29 | 2018-08-29 | Heating device for high-temperature thin film deposition of thin metal |
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| CN201810995176.3A CN109097756B (en) | 2018-08-29 | 2018-08-29 | Heating device for high-temperature thin film deposition of thin metal |
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| CN109097756B true CN109097756B (en) | 2020-10-23 |
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| CN1156602C (en) * | 2001-03-30 | 2004-07-07 | 中国科学院物理研究所 | Heating method for preparing metal substrate film |
| TWI590701B (en) * | 2012-03-26 | 2017-07-01 | 劉忠男 | High frequency electric heating rolling belt |
| 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 |
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