CN108396294B - Film deposition system and control method - Google Patents

Film deposition system and control method Download PDF

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Publication number
CN108396294B
CN108396294B CN201810077393.4A CN201810077393A CN108396294B CN 108396294 B CN108396294 B CN 108396294B CN 201810077393 A CN201810077393 A CN 201810077393A CN 108396294 B CN108396294 B CN 108396294B
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film deposition
thin film
vacuum
sample transfer
deposition system
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CN108396294A (en
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袁洁
何格
张旭
魏忠旭
金魁
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Institute of Physics of CAS
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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
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/24Vacuum evaporation
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • 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

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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)
  • Physical Vapour Deposition (AREA)

Abstract

The invention relates to a film deposition system and a control method, wherein the film deposition system comprises: the film deposition cavity is used for preparing a film; a sample transfer cavity for providing a channel for sample transfer; the vacuumizing device is used for vacuumizing; the vacuum pipeline is provided with a first port connected with the film deposition cavity, a second port connected with the sample transfer cavity and a third port connected with the vacuumizing device, a first valve is arranged at the first port, and a second valve is arranged at the second port; and a sample transfer rod mounted on the sample transfer chamber and configured to be movable along the sample transfer chamber, the vacuum pipe, and the thin film deposition chamber. The film deposition system can be connected with various types of film growth equipment or film measurement equipment to realize film growth or film measurement of a sample in a high vacuum state, and can be transferred to a required working place, so that the film deposition system is convenient to use.

Description

Film deposition system and control method
Technical Field
The invention relates to a film deposition system and a control method, in particular to a movable film deposition system capable of working in a high-vacuum environment and a control method.
Background
Film deposition is a series of processes involving the adsorption of atoms, diffusion of adsorbed atoms at the surface, and coalescence at appropriate locations to gradually form and grow a film. Thin film deposition has been widely used for surface treatment of various objects such as jewels, tableware, tools, molds, or semiconductor elements, and homogeneous or heterogeneous thin films are formed on the surfaces of the objects to improve wear resistance, heat resistance, corrosion resistance, and the like. Depending on the deposition technique and process parameters, the deposited film may have a single crystal, polycrystalline or amorphous structure. Thin film deposition techniques generally fall into two broad categories, physical vapor deposition and chemical vapor deposition. Chemical vapor deposition, which comprises normal pressure chemical vapor deposition, low pressure chemical vapor deposition and plasma-assisted chemical vapor deposition according to the development process of chemical vapor deposition, and the product is deposited on the surface of a wafer; physical vapor deposition, also known as metal plating, includes: vapor deposition, which is a process of depositing a thin film by utilizing the saturated vapor pressure of the vapor deposition object at high temperature (close to the melting point); sputtering, in which ions bombard the electrode of the sputtering object to make the vapor phase have the particles (such as atoms) of the object to be plated, so as to deposit the film.
In the physical properties in a condensed state or other studies, it is often required that a measurement sample is grown and measured without being exposed to the atmosphere. However, most surface sensitive thin film measurements cannot be performed in a vacuum environment, which results in measurement of only easily cleaved single crystal samples, greatly limiting the measurement range.
Disclosure of Invention
In view of the above, the present invention provides a thin film deposition system that can be connected to a thin film growth apparatus or a thin film measurement apparatus, and that operates in a high vacuum state and is easily moved.
According to an aspect of the present invention, there is provided a thin film deposition system including: the film deposition cavity is used for preparing a film; a sample transfer cavity for providing a channel for sample transfer; the vacuumizing device is used for vacuumizing; the vacuum pipeline is provided with a first port connected with the film deposition cavity, a second port connected with the sample transfer cavity and a third port connected with the vacuumizing device, a first valve is arranged at the first port, and a second valve is arranged at the second port; and a sample transfer rod mounted on the sample transfer chamber and configured to be movable along the sample transfer chamber, the vacuum pipe, and the thin film deposition chamber.
Preferably, the vacuum conduit further comprises a fourth port for connection to a vacuum measurement device.
Preferably, the vacuum measuring device includes: and the vacuum gauge is used for measuring the vacuum degree in the film deposition cavity.
Preferably, the thin film deposition chamber is a spherical chamber.
Preferably, the film deposition chamber adopts at least one of magnetron sputtering, pulsed laser deposition and molecular beam epitaxy to prepare the film.
Preferably, an ion pump is arranged in the sample transfer cavity for maintaining the vacuum degree during the sample transfer process.
Preferably, a sample storage rack capable of storing a plurality of samples simultaneously is further arranged inside the sample transfer cavity.
Preferably, the sample storage rack comprises: the sample transfer device comprises a platform and an adjusting rod connected with the platform, wherein one part of the adjusting rod is positioned outside a sample transfer cavity and used for adjusting the height of the platform and rotating the platform.
Preferably, the thin film deposition system further comprises: the mobile vehicle is provided with a vehicle body, a handrail and a support, wherein the handrail and the support are installed on the vehicle body, and the film deposition cavity, the sample transfer cavity and the vacuum pipeline are installed on the support.
Preferably, an uninterruptible power supply UPS is further disposed on the moving vehicle, and is used for supplying power to the thin film deposition system.
Preferably, the thin film deposition system further comprises: a thin film growth apparatus or a thin film measurement apparatus.
According to another aspect of the present invention, there is provided a method of controlling a thin film deposition system, comprising: opening a first valve of the thin film deposition system and closing a second valve; starting a vacuumizing device; when the vacuum degree in the film deposition chamber reaches a preset standard, closing a first valve of the film deposition system, and opening a second valve; and when the vacuum degree in the sample transfer cavity reaches a preset standard, closing the vacuumizing device.
The film deposition system can realize in-situ growth and transfer of film deposition in a high-vacuum working environment.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in detail embodiments thereof with reference to the attached drawings. It is to be understood that the drawings in the following description are directed to only one embodiment of the invention and are not intended as a limitation on the invention.
FIG. 1 is a schematic diagram of a thin film deposition system according to the present invention;
FIG. 2 is a control method of the thin film deposition system of the present invention.
Detailed Description
The invention will be described in more detail below with reference to the accompanying drawings. Like parts are designated with like reference numerals throughout the various figures. For purposes of clarity, the various features in the drawings are not necessarily drawn to scale. In addition, certain well known components may not be shown.
Numerous specific details of the invention are set forth in the following description in order to provide a more thorough understanding of the invention. However, as will be understood by those skilled in the art, the present invention may be practiced without these specific details.
As shown in fig. 1, in the film system design diagram of the present invention, the first port 101 of the vacuum pipe 1 is connected to the film deposition chamber 2, and the film deposition chamber 2 may adopt at least one of magnetron sputtering, pulsed laser deposition, and molecular beam epitaxy methods to perform film preparation. And the on-off of the vacuum pipeline 1 and the film deposition chamber 2 is controlled by the first valve 3. The film deposition cavity 2 is a spherical cavity, and the design can save space on one hand and save time required by vacuumizing on the other hand. The working module 20 in the figure may be a thin film growth apparatus 201 for performing thin film deposition growth. The second port 102 in the vacuum tubing 1 is connected to the sample transfer chamber 5, the sample transfer chamber 5 providing a passage for sample transfer. And the second valve 4 is used for controlling the connection and disconnection of the vacuum pipeline 1 and the sample transfer cavity 5. The sample transfer chamber 5 has a sample storage rack 510 for storing a plurality of samples while transferring the samples, and the sample storage rack 510 includes a platform 511 and an adjustment lever 512 connected to the platform 511, and a portion of the adjustment lever 512 is located outside the sample transfer chamber for adjusting the height and rotating the platform 511. The sample transfer chamber 5 also has an ion pump (not shown) therein, which maintains the vacuum level of the vacuum environment generated by a vacuum pumping device (not shown) connected to the fourth port 104 of the vacuum pipe 1 during the transfer of the system by the carriage 7. The third port 103 of the vacuum pipe 1 can be connected to a vacuum pumping device, such as a vacuum pump set, which can pump air in the vacuum pipe 1 and other connection parts of the thin film deposition system into a vacuum state to provide a vacuum environment for the operation of the thin film deposition system of the present invention. The fourth port 104 in the vacuum pipe 1 may be connected to a vacuum measuring device (not shown), which may be a vacuum gauge, for measuring the degree of vacuum in the thin film deposition system.
The vacuum degree refers to the gas rarefied degree of the system in the vacuum state; if the pressure in the equipment to be measured is lower than the atmospheric pressure, a vacuum measuring device is required to be installed for pressure measurement, and the value read by the vacuum measuring device is called vacuum degree; the vacuum value is a value indicating that the actual value of the system pressure is lower than the atmospheric pressure, that is: the vacuum degree is atmospheric pressure-absolute pressure, and the absolute pressure is atmospheric pressure + gauge pressure. There are generally two methods for the identification of the degree of vacuum: firstly, the pressure is marked by absolute pressure and absolute vacuum degree (namely, the pressure is higher than theoretical vacuum); in practical situation, the absolute pressure value of the vacuum pump set is between 0 KPa and 101.325 KPa. The absolute pressure value is measured by an absolute pressure meter, and at 20 ℃ and an altitude equal to 0, the initial value of the meter for measuring the vacuum degree (absolute vacuum meter) is 101.325KPa (i.e., one standard atmospheric pressure). The second is identified by "relative pressure" and "relative vacuum" (i.e., how much pressure is lower than "atmospheric pressure"). The "relative degree of vacuum" refers to a difference between the pressure of the object to be measured and the atmospheric pressure at the measurement site. Measured with a common vacuum gauge. In the absence of vacuum (i.e., at atmospheric pressure), the initial value of the ordinary vacuum gauge is 0. When vacuum is measured, it has a value between 0 and-101.325 KPa (typically expressed as a negative number). For example, a micro vacuum pump having a PH2506B measuring-75 KPa indicates that the pump can draw a vacuum level 75KPa below atmospheric pressure at the measurement site. The vacuum measuring device in the system is a vacuum gauge or any other type of vacuum measuring device which can be used for the purpose.
The thin film deposition system also comprises a sample transmission rod 6 connected with the sample transmission cavity 5, and the sample transmission rod 6 can move in the sample transfer cavity 5, the vacuum pipeline 1 and the thin film deposition cavity 2 in the thin film deposition system. Specifically, a sample to be grown or measured can be sent to the thin film deposition chamber 2 or taken out from the thin film deposition chamber 2. According to fig. 1, the vacuum pipe 1, the thin film deposition chamber 2, the thin film growth apparatus 201, the sample transfer chamber 5, and the sample transfer rod 6 should be at the same height, so as to facilitate the practical operation and use of the thin film deposition system of the present invention. The moving vehicle 7 comprises a vehicle body 710, and a handrail 720 and a support 730 which are mounted on the vehicle body, and is connected with and supports the thin film deposition chamber 2, the vacuum pipe 1 and the sample transfer chamber 5 in the thin film deposition system through the support 730 (which can be divided into 731, 732, 733). An Uninterruptible Power Supply (UPS) is also installed on the mobile vehicle 7 to provide Power support for the short-distance transport film deposition system of the mobile vehicle 7.
The UPS is a system device that connects a storage battery (mostly a lead-acid maintenance-free storage battery) with a host and converts dc power into commercial power through a module circuit such as a host inverter. The UPS is mainly used to provide a stable and uninterrupted power supply to a single computer, a computer network system, or other power electronic devices such as solenoid valves, pressure transmitters, etc. When the commercial power input is normal, the UPS supplies the commercial power to the load for use after stabilizing the voltage, and the UPS is an alternating current type voltage stabilizer and also charges the battery in the machine; when the commercial power is interrupted (power failure in accident), the UPS immediately supplies the direct current electric energy of the battery to the load by a method of switching and converting the inverter to continuously supply 220V alternating current to the load, so that the load keeps normal work and the software and hardware of the load are protected from being damaged. UPS devices typically provide protection against either excessive voltage or insufficient voltage. The UPS power source in the vehicle 7 in the present system may be any kind of UPS power source.
As shown in FIG. 1, the operation module may be a thin film measuring apparatus 202, and the thin film measuring apparatus 202 is connected to the thin film deposition chamber 2 to measure a parameter related to the thin film. The thin film measurement device 202 may be any measurement instrument selected according to actual measurement requirements, such as a scanning tunneling electron microscope, an angle-resolved photoelectron spectroscopy. The connection relationship of other parts in the film deposition system is unchanged. A first port 101 in the vacuum pipeline 1 is connected with the thin film deposition cavity 2, a second port 102 in the vacuum pipeline 1 is connected with the sample transfer cavity 5, a third port 103 of the vacuum pipeline 1 is connected with a vacuumizing device for realizing the vacuum environment of the thin film deposition system, and a fourth port 104 of the vacuum pipeline 1 is connected with a vacuum measuring device for measuring the vacuum degree; a first valve 3 positioned on the vacuum pipeline 1 controls the on-off of the vacuum pipeline 1 and the thin film deposition cavity 2, and a second valve 4 positioned on the vacuum pipeline 1 controls the on-off of the vacuum pipeline 1 and the sample transmission cavity 5; the sample transfer rod 6 connected with the sample transfer cavity 5 can move in the sample transfer cavity 5, the vacuum pipeline 1 and the film deposition cavity 2; the moving vehicle 7 is respectively connected with the thin film deposition chamber 2, the vacuum pipeline 1 and the sample transfer chamber 5 through a support 730 (which can be divided into 731, 732 and 733) on the vehicle body 710, and provides support for the whole thin film deposition system. Similarly, the sample transfer rod 6, the sample transfer chamber 5, the vacuum pipeline 1, the thin film deposition chamber 2 and the thin film measurement device 202 should be at the same height, which is suitable for the system operation and practical operation.
The vacuum state in the working state of the system, which is realized by the vacuum pumping device connected with the third port 103 of the vacuum pipeline 1, provides a high vacuum working environment of the whole system, and achieves the purpose of the invention design of the system. The thin film system of the present invention is connected to the thin film growth apparatus 201 or the thin film measurement apparatus 202 to cause the system to perform specific work content. The thin film growth apparatus 201 or the thin film measurement apparatus 202 may be any one of the types of apparatuses described above. As shown in FIG. 2, the control method of the thin film deposition system of the present invention is as follows:
in step S801, the thin film growth apparatus 201 or the thin film measurement apparatus 202 is connected to the thin film deposition chamber 2.
In step S802, the second valve 4 is closed, and the first valve 3 is opened.
Step S803, after the two valves are confirmed to be correct, the vacuum pumping device connected to the third port 103 of the vacuum pipe 1 is turned on until the vacuum degree in the film deposition chamber 2 reaches a predetermined standard. The degree of vacuum can be confirmed by observing the vacuum measuring device connected to the fourth port 104 connected to the vacuum pipe 1.
And 803, after confirming that the film deposition chamber 2 reaches the vacuum degree of the preset standard, closing the first valve 3 and opening the second valve 4.
And step 804, after the states of the two valves are confirmed to be correct, and when the vacuum degree in the sample transfer cavity 5 reaches a preset standard, closing the vacuumizing device. Likewise, the degree of vacuum can be confirmed by observing the vacuum measuring device connected to the fourth port 104 connected to the vacuum pipe 1.
Through the five steps, the high vacuum environment required by the operation of the thin film deposition system can be obtained. If the system work site needs to be changed, the push-pull vehicle 7 is moved to the work site. During the transfer of the trolley 7, the ion pump in the sample transfer chamber 5 can be turned on to maintain a vacuum environment in the system.
The film deposition system can realize two works of film growth and film measurement, the high vacuum state of the system provides a reliable and convenient working environment for research of condensed physical properties and the like, and the added movable vehicle is convenient for the working system to be transferred to any working place needing to be reached.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
While embodiments in accordance with the invention have been described above, these embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments described. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention and various embodiments with various modifications as are suited to the particular use contemplated. The invention is limited only by the claims and their full scope and equivalents.

Claims (10)

1. A thin film deposition system, wherein the thin film deposition system comprises:
the film deposition cavity is used for preparing a film;
a sample transfer cavity for providing a channel for sample transfer;
the vacuumizing device is used for vacuumizing;
the vacuum pipeline is provided with a first port connected with the film deposition cavity, a second port connected with the sample transfer cavity and a third port connected with the vacuumizing device, a first valve is arranged at the first port, and a second valve is arranged at the second port;
the sample transmission rod is arranged on the sample transfer cavity; and
a moving vehicle having a vehicle body, and a handrail and a support mounted on the vehicle body, the thin film deposition chamber, the sample transfer chamber, and the vacuum duct being mounted on the support,
wherein the thin film deposition chamber, the sample transfer chamber, the vacuum conduit, and the sample transfer rod are at equal heights such that the sample transfer rod is movable along the sample transfer chamber, the vacuum conduit, and the thin film deposition chamber,
when the moving vehicle moves to the film growth equipment, the film deposition cavity is connected with the film growth equipment to realize film growth, when the moving vehicle moves to the film measurement equipment, the film deposition cavity is connected with the film measurement equipment to realize film measurement, and the vacuumizing device is connected with the third port to provide a vacuum state in a working state.
2. The thin film deposition system of claim 1, wherein the vacuum line further comprises a fourth port for connection to a vacuum measurement device.
3. The thin film deposition system of claim 2, wherein the vacuum measurement device comprises: and the vacuum gauge is used for measuring the vacuum degree in the film deposition cavity.
4. The thin film deposition system of claim 1, wherein the thin film deposition chamber is a spherical chamber.
5. The thin film deposition system of claim 1, wherein the thin film deposition chamber employs at least one of magnetron sputtering, pulsed laser deposition, and molecular beam epitaxy for thin film preparation.
6. The thin film deposition system of claim 1, wherein an ion pump is disposed inside the sample transfer chamber for maintaining a vacuum during sample transfer.
7. The thin film deposition system according to claim 1, wherein a sample storage rack for storing a plurality of samples simultaneously is further provided inside the sample transfer chamber.
8. The thin film deposition system of claim 7, wherein the sample holder comprises: the sample transfer device comprises a platform and an adjusting rod connected with the platform, wherein one part of the adjusting rod is positioned outside a sample transfer cavity and used for adjusting the height of the platform and rotating the platform.
9. The thin film deposition system as claimed in claim 8, wherein an Uninterruptible Power Supply (UPS) is further provided on the mobile cart for supplying power to the thin film deposition system.
10. A control method of the thin film deposition system according to any one of claims 1 to 9, comprising:
the thin film growth equipment or the thin film measurement equipment is connected with the thin film deposition system;
opening a first valve of the thin film deposition system and closing a second valve;
starting a vacuumizing device;
when the vacuum degree in the film deposition chamber reaches a preset standard, closing a first valve of the film deposition system, and opening a second valve;
and when the vacuum degree in the sample transfer cavity reaches a preset standard, closing the vacuumizing device.
CN201810077393.4A 2018-01-26 2018-01-26 Film deposition system and control method Active CN108396294B (en)

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CN109207949B (en) * 2018-10-23 2020-06-16 宁波工程学院 Method for plating non-uniform multilayer film
CN109580325B (en) * 2018-11-17 2023-08-29 金华职业技术学院 Method for preparing film sample by deposition
CN114965866B (en) * 2021-02-24 2023-09-08 中国科学院物理研究所 System for measuring physical properties of a material
CN113447513A (en) * 2021-06-29 2021-09-28 哈尔滨工业大学 Long-acting vacuum transfer sample stage for X-ray photoelectron spectrometer and transfer method

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JP3268394B2 (en) * 1992-03-11 2002-03-25 東京エレクトロン株式会社 Processing method
JP3967424B2 (en) * 1997-04-30 2007-08-29 東京エレクトロン株式会社 Vacuum processing apparatus and pressure adjustment method
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