A high-vacuum electron beam evaporation thin film deposition device

By combining the plug-in valve connection of the evaporation and oxidation device in the high-vacuum electron beam evaporation film equipment, the stage rotation and cooling, and the film thickness online monitoring, the problem that existing equipment cannot perform oblique angle coating, oxidation and etching is solved, and the preparation of high-quality complex structural films is achieved.

CN116377398BActive Publication Date: 2025-07-29SOUTHWEST JIAOTONG UNIV +1
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Patent Information

Application Number
CN202310327588.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-03-30
Publication Date
2025-07-29
Estimated Expiration
2043-03-30

AI Technical Summary

Technical Problem

The existing high-vacuum electron beam evaporation film equipment cannot perform oblique angle coating, film oxidation and ion etching, and the film thickness quality control is limited, so the preparation of complex structural films cannot be achieved.

Method used

A high-vacuum electron beam evaporation film deposition equipment is designed, and the evaporation device and oxidation device are connected through a plug-in valve. Combined with the stage rotation and cooling functions, it is equipped with a Kaufman ion source and film thickness online monitoring system to realize oblique angle coating, online oxidation and etching to ensure film thickness uniformity and quality.

Benefits of technology

It realizes high-quality preparation of complex structural films, has online film thickness monitoring and control capabilities, and improves film layer uniformity and film formation efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a high-vacuum electron beam evaporation thin film deposition device, which includes a device support, an evaporation device mounted on the device support, an oxidation device connected to the evaporation device through a gate valve, and a vacuum system for evacuating the evaporation device and the oxidation device. The oxidation device includes an oxidation chamber, a carrier mechanism rotatably mounted on the oxidation chamber, and an in-situ thickness monitoring system. A Kaufman ion source is also mounted on the oxidation chamber. The present invention connects the evaporation device and the oxidation device together through a gate valve, enabling the device to combine electron beam evaporation, in-situ oxidation, and in-situ etching functions; it can realize continuous operations of sample coating, etching, and oxidation, and prepare thin film samples with complex structures and high quality.
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Description

Technical Field

[0001] The present invention belongs to the technical field of material processing equipment, and relates to an electron beam evaporation coating equipment, in particular to a high-vacuum electron beam evaporation thin film deposition equipment. Background Art

[0002] Vacuum coating technology originated in the 1930s and began large-scale production in the late 1970s. It has now been widely used in fields such as acid resistance, corrosion resistance, heat resistance, surface hardening, decoration, lubrication, optoelectronic communication, electronic integration, and energy.

[0003] Vacuum coating equipment mainly refers to a type of coating that needs to be carried out under a relatively high vacuum. Specifically, it includes many types, including vacuum ion evaporation, magnetron sputtering, MBE molecular beam epitaxy, PLD laser sputtering deposition, etc. Evaporation coating generally heats the target material so that the surface components are evaporated in the form of atomic clusters or ions. And settle on the surface of the substrate, and form a thin film through the film formation process (scattered dots - island structure - maze structure - layer growth). To complete vacuum coating, two conditions must be met: first, there must be conditions to create a high vacuum; second, the mean free path of the film material vapor molecules must be greater than the distance from the evaporation source to the workpiece, that is, there must be a sufficiently long mean free path of molecules (the statistical average of the distance that molecules fly over between two consecutive collisions with other molecules). For the formed thin film, its uniformity refers to the situation where the film thickness deposited on the substrate to be coated changes with the position of the substrate in the vacuum chamber. It is an important indicator to measure the quality of the thin film and the performance of the coating device. The principle of electron beam evaporation coating is to use the huge thermal energy provided by the electron gun to melt the metal or non-metal in the crucible. When the saturated vapor pressure is reached, it is evaporated onto the surface of the ion-bombarded clean sample to achieve the coating process.

[0004] Electron beam evaporation is widely used in various applications due to its high deposition rate and high material utilization efficiency. For example, the high-performance aerospace and automotive industries have high requirements for the high temperature resistance and wear resistance of materials; durable tool hard coatings; and chemical barriers and coatings to protect surfaces in corrosive environments. Electron beam evaporation is also used in optical thin films, including laser optics, solar panels, glass, and architectural glass, to endow them with the required conductive, reflective, and transmissive properties.

[0005] Electron beam evaporation can evaporate high-melting-point materials and has higher efficiency than general resistance heating evaporation. Electron beam evaporation can be widely used in optical coatings such as high-purity thin films and conductive glass. It also has potential industrial applications for wear-resistant and thermal barrier coatings in the aerospace industry and hard coatings in the cutting and tool industry. However, electron beam evaporation cannot be used to coat the inner surfaces of complex geometries. In addition, filament degradation in the electron gun may cause uneven evaporation rates.

[0006] Existing high-vacuum electron beam evaporation thin film equipment, such as DZS500, although it can achieve a relatively high vacuum degree and can prepare high-quality thin films, still has the following problems: (1) It is unable to perform oblique angle coating; (2) It is unable to oxidize the thin film; (3) Due to the absence of a Kaufman ion source, it is unable to perform the ion beam etching (IBE) process; (4) The film thickness quality control is mainly one-dimensional thickness monitoring, and it is unable to achieve on-line monitoring of the film thickness under the condition of gradually changing thickness. Summary of the Invention

[0007] The purpose of the present invention aims at the problems existing in the above-mentioned existing technologies, and provides a high-vacuum electron beam evaporation thin film deposition equipment, which can achieve oblique angle coating, and can realize on-line oxidation and on-line film thickness monitoring of the thin film, and improve the film formation quality by adjusting the cooling method of the stage.

[0008] In order to achieve the above purpose, the present invention adopts the following technical means to realize.

[0009] The high-vacuum electron beam evaporation thin film deposition equipment provided by the present invention includes: an equipment bracket, a vapor deposition device installed on the equipment bracket, an oxidation device connected to the vapor deposition device through a gate valve, and a vacuum system for evacuating the vapor deposition device and the oxidation device;

[0010] The above-mentioned oxidation device includes an oxidation chamber and a stage mechanism rotatably installed on the oxidation chamber; the oxidation chamber is connected to the vacuum system through a pipeline; the oxidation chamber is provided with opposite first installation interfaces and second installation interfaces; the first installation interface is connected to the gate valve, and the second installation interface is used for installing a film thickness gauge probe; the stage mechanism includes a stage and a rotating shaft fixedly connected to the stage; the stage is located between the first installation interface and the second installation interface; a liquid circulation channel is provided inside the stage, the rotating shaft is hollow, and an inner pipe communicating with the internal circulation channel of the stage is provided, and the inner pipe divides the cavity of the rotating shaft into a liquid inlet channel and a liquid outlet channel; a Kaufman ion source is also installed on the oxidation chamber, and the sputtering range of the Kaufman ion source covers the stage; the oxidation device also includes an on-line monitoring system for monitoring the thickness of the thin film after deposition.

[0011] The vacuum system includes a first vacuum device for evacuating the vapor deposition device and a second vacuum device for evacuating the oxidation device.

[0012] The above-mentioned high-vacuum electron beam evaporation thin film deposition equipment connects the vapor deposition device and the oxidation device together through a gate valve, and has functions such as electron beam evaporation, oxidation, etching, etc., and can also realize the rotation of the stage, so as to realize on-line evaporation, oxidation, etching, etc. of the sample, and can realize precise control of the film thickness, thereby providing an effective way for preparing high-quality complex structure thin films (such as Josephson junctions).

[0013] The above-mentioned high-vacuum electron beam evaporation thin film deposition equipment, the evaporation device includes a vacuum chamber; a crucible for holding the raw material to be plated, a baffle for blocking the opening of the crucible and a baffle controller, an electron gun for heating the crucible, and an electron gun power supply for controlling the electron gun are arranged in the vacuum chamber. A first vacuum interface and a third mounting interface are arranged on the vacuum chamber; the first vacuum device includes a first molecular pump and a first mechanical pump; the first molecular pump is connected to the first vacuum interface through a first high-vacuum valve; the first mechanical pump is connected to the first vacuum interface and the first molecular pump through pipelines respectively via two low-vacuum valves; the third mounting interface is connected to a gate valve. The first vacuum interface is also provided with a resistance gauge and an ionization gauge for measuring low vacuum and high vacuum. The vacuum chamber is provided with a hinged vacuum chamber door, and an observation window is arranged on the vacuum chamber door.

[0014] The above-mentioned high-vacuum electron beam evaporation thin film deposition equipment, a second vacuum interface is arranged on the oxidation chamber; the second vacuum device includes a second molecular pump and a second mechanical pump; the second molecular pump is connected to the second vacuum interface through a second high-vacuum valve; the second mechanical pump is connected to the second vacuum interface and the second molecular pump through pipelines respectively via two low-vacuum valves. The second vacuum interface is also provided with a resistance gauge and an ionization gauge for measuring low vacuum and high vacuum. The oxidation chamber is provided with an observation window.

[0015] The above-mentioned high-vacuum electron beam evaporation thin film deposition equipment, one or more gas interfaces can also be arranged on the oxidation chamber and connected to corresponding gas supply devices (such as oxygen, argon supply devices, etc.).

[0016] The above-mentioned high-vacuum electron beam evaporation thin film deposition equipment, the loading mechanism has both rotation and cooling functions. In order to ensure the sealing effect of the oxidation chamber, the sealing between the rotating shaft and the oxidation chamber is achieved through magnetic fluid. For this purpose, the loading mechanism further includes a magnetic fluid chamber sleeved outside the rotating shaft; the magnetic fluid chamber is connected to the loading platform interface arranged on the oxidation chamber through a flange; magnetic fluid is encapsulated in the magnetic fluid chamber. A bearing seat adapted to the rotating shaft is arranged inside the magnetic fluid chamber; a liquid inlet and a liquid outlet respectively connected to the liquid inlet channel and the liquid outlet channel are arranged on the rotating shaft, and a rotating handwheel is further arranged at the end of the rotating shaft. The present invention uses liquid nitrogen as the coolant.

[0017] The above-mentioned high-vacuum electron beam evaporation thin film deposition equipment, in order to control the rotation of the loading platform, the loading mechanism is further provided with a limit pin, and the limit pin passes through the rotating handwheel along the direction parallel to the axial direction of the rotating shaft and penetrates into the magnetic fluid chamber; the limit pin is threadedly connected to the rotating handwheel and the magnetic fluid chamber.

[0018] The above-mentioned high-vacuum electron beam evaporation thin film deposition equipment, a substrate holder is arranged on the loading platform and is pressed by a pressing plate fixedly connected to the loading platform.

[0019] For the above high-vacuum electron beam evaporation thin film deposition equipment, in order to uniformly heat the sample on the stage, a heating device can be provided in the oxidation chamber; the specific structure of the heating device does not fall within the protection scope of the present invention, and conventional heating methods in the art can be adopted. For example, an electric heating rod can be installed in the oxidation chamber, or a number of heating wires can be uniformly arranged axially along the inner wall of the oxidation chamber, or a number of heating wires can be uniformly arranged circumferentially along the inner wall of the oxidation chamber.

[0020] For the above high-vacuum electron beam evaporation thin film deposition equipment, the film thickness gauge probe is installed on the cover plate at the top of the oxidation chamber; the cover plate is detachably connected to the oxidation chamber. In the present invention, the evaporation rate (m (g / s)) of the evaporation raw material is obtained through a film thickness controller, and then the film layer thickness of the sample on the stage is calculated according to the following formula:

[0021] (1) When the stage is parallel to the horizontal plane and the middle position of the stage is opposite to the evaporation raw material, the film thickness t0 at the middle position of the stage is:

[0022] t0 = m / 4πρh 2

[0023] In the formula, ρ represents the density of the evaporation raw material, and h represents the distance between the middle position of the stage and the evaporation raw material.

[0024] The film thickness t at a position x on the stage away from its middle position is:

[0025]

[0026] (2) When the stage forms an angle α with the horizontal plane and the middle position of the stage is opposite to the evaporation raw material, the film thickness t'0 at the middle position of the stage is:

[0027] t'0 = t0 cosα

[0028] The film thickness t' at any x position (the angle deviating from the middle position is θ) in the direction from the middle position of the stage towards the evaporation raw material is:

[0029]

[0030] The film thickness t'' at any x position (the angle deviating from the middle position is θ') in the direction from the middle position of the stage away from the evaporation raw material is:

[0031]

[0032] The on-line thickness monitoring system includes an oscillator connected to the thickness gauge probe, a film thickness controller connected to the oscillator, and an electron gun power supply and a baffle controller connected to the film thickness controller. The thickness gauge probe and the oscillator form an oscillation circuit. As the thickness of the coating on the surface of the thickness gauge probe changes, the frequency value of the oscillation circuit changes. The film thickness controller can obtain the evaporation rate of the evaporation raw material based on the changed oscillation frequency value; based on the obtained evaporation rate and the density of the evaporation raw material, the evaporation film thickness distribution of the sample being plated or obliquely plated (along the inclination angle of the stage) is calculated according to the above formula. When the evaporation film thickness distribution meets the set requirements, the electron gun power supply for heating the raw material to be evaporated is controlled to turn off, and at the same time, the baffle is controlled to be placed above the evaporation raw material through the baffle controller.

[0033] The high-vacuum electron beam evaporation thin film deposition equipment provided by the present invention has the following outstanding beneficial effects compared with the prior art:

[0034] 1. The present invention connects the evaporation device and the oxidation device through a gate valve, enabling the equipment to combine the functions of electron beam evaporation, on-line oxidation and on-line etching; it can realize continuous operations of sample coating, etching and oxidation, and prepare thin film samples with complex structures and high quality;

[0035] 2. The present invention can simultaneously realize the rotation and cooling of the stage. By rotating the stage, oblique angle coating can be achieved;

[0036] 3. The stage mechanism of the present invention uses a liquid nitrogen cooling method based on magnetic fluid, which can effectively improve the film layer quality;

[0037] 4. The present invention is equipped with an on-line thickness monitoring system, which can monitor the thickness of the prepared film layer in real time, and thus accurately control the thickness of the prepared thin film sample. Description of the Drawings

[0038] Figure 1 It is the front view of the high-vacuum electron beam evaporation thin film deposition equipment provided by the embodiment of the present invention.

[0039] Figure 2 It is the three-dimensional view of the high-vacuum electron beam evaporation thin film deposition equipment provided by the embodiment of the present invention.

[0040] Figure 3 It is the structural schematic diagram of the evaporation device provided by the embodiment of the present invention.

[0041] Figure 4 It is the structural schematic diagram of the oxidation device provided by the embodiment of the present invention.

[0042] Figure 5 It is the structural schematic diagram of the stage mechanism provided by the embodiment of the present invention.

[0043] Figure 6Schematic diagram of the principle of the on-line thickness monitoring system provided by the embodiment of the present invention.

[0044] Figure 7 Schematic diagram of the principle of film thickness distribution in the embodiment of the present invention.

[0045] In the figure, 1 - equipment support, 2 - evaporation device, 21 - vacuum chamber, 211 - first vacuum interface, 212 - third installation interface, 213 - vacuum chamber door, 214 - crucible, 215 - baffle controller, 216 - electron gun power supply, 3 - oxidation device, 31 - oxidation chamber, 311 - first installation interface, 312 - second installation interface, 313 - second vacuum interface, 314 - cover plate, 32 - loading mechanism, 321 - loading platform, 3211 - substrate holder, 3212 - pressing plate, 322 - rotating shaft, 3221 - liquid inlet, 3222 - liquid outlet, 3223 - rotating handwheel, 323 - inner tube, 324 - magnetohydrodynamic chamber, 325 - limit pin, 33 - film thickness gauge probe, 34 - Kaufman ion source, 35 - oscillator, 36 - film thickness controller, 4 - gate valve, 5 - vacuum system, 51 - first vacuum device, 511 - first molecular pump, 512 - first mechanical pump, 513 - first high vacuum valve, 514, 515 - low vacuum valves, 52 - second vacuum device, 521 - second molecular pump, 522 - second mechanical pump, 523 - second high vacuum valve. Detailed implementation manners

[0046] The present invention will be specifically described below through embodiments. It is necessary to point out here that these embodiments are only used to further illustrate the present invention and should not be construed as limiting the protection scope of the present invention. Those skilled in the art can make some non-essential improvements and adjustments based on the content of the present invention above.

[0047] Embodiment 1

[0048] The high-vacuum electron beam evaporation thin film deposition equipment provided by this embodiment, as Figure 1 and Figure 2 shown, includes: an equipment support 1, an evaporation device 2 installed on the equipment support 1, an oxidation device 3 connected to the evaporation device 2 through a gate valve 4, and a vacuum system 5 for evacuating the evaporation device 2 and the oxidation device 3.

[0049] As Figure 1 and Figure 2 shown, the vacuum system 5 includes a first vacuum device 51 for evacuating the evaporation device 2 and a second vacuum device 52 for evacuating the oxidation device 3. The first vacuum device 51 includes a first molecular pump 511 and a first mechanical pump 512. The second vacuum device 52 includes a second molecular pump 521 and a second mechanical pump 522.

[0050] AsFigures 1 to 3 As shown in the figure, the evaporation device 2 includes a vacuum chamber 21; inside the vacuum chamber 21, there are provided a crucible 214 for containing the raw material to be plated, a baffle for blocking the opening of the crucible and a baffle controller 215, an electron gun for heating the crucible, and an electron gun power supply 216 for controlling the electron gun. The vacuum chamber 21 is provided with a vacuum chamber door 213 hinged thereto. The vacuum chamber door and the vacuum chamber 21 can be hinged together with a hinge as the door hinge mechanism. In order to increase the sealing performance between the vacuum chamber door 213 and the vacuum chamber 21, the two can be further locked by clamping, flanges, etc. An observation window is provided on the vacuum chamber door, which is convenient for the operator to observe the evaporation situation of the raw material to be evaporated in the crucible. The vacuum chamber 21 is provided with a first vacuum interface 211 and a third installation interface 212; the first molecular pump 511 is connected to the first vacuum interface 211 through a pipeline via a first high-vacuum valve 513; the first mechanical pump 512 is connected to the first vacuum interface 211 and the first molecular pump 511 through pipelines via two low-vacuum valves (514, 515) respectively; the third installation interface 212 is connected to the gate valve 4. Specifically, a gate valve interface is first welded to the third installation interface, and then the gate valve interface is hermetically connected to the gate valve. The first vacuum interface 211 is also provided with a resistance gauge and an ionization gauge for measuring low vacuum and high vacuum. In addition, a resistance gauge is also provided on the pipeline connected to the first mechanical pump.

[0051] As Figure 1 , Figure 2 , Figure 4 As shown in the figure, the oxidation device 3 includes an oxidation chamber 31, a loading mechanism 32 rotatably installed on the oxidation chamber 31, and an in-line thickness monitoring system.

[0052] The oxidation chamber 31 is provided with opposite first installation interface 311 and second installation interface 312. The first installation interface 311 is hermetically connected to the gate valve 4, and the second installation interface is used to connect to a cover plate 314 for installing a film thickness gauge probe 33. The oxidation chamber 31 is provided with a second vacuum interface 313. The second molecular pump 521 is connected to the second vacuum interface 313 through a pipeline via a second high-vacuum valve 523; the second mechanical pump 522 is connected to the second vacuum interface 313 and the second molecular pump 521 through pipelines via two low-vacuum valves respectively. The second vacuum interface 211 is also provided with a resistance gauge and an ionization gauge for measuring low vacuum and high vacuum. In addition, a resistance gauge is also provided on the pipeline connected to the second mechanical pump. Two gas interfaces are also provided on the top cover plate 314 of the oxidation chamber 31, which are connected to corresponding gas supply devices (such as oxygen, argon supply devices, etc.).

[0053] As Figure 5As shown in the figure, the loading mechanism 32 includes a loading platform 321, a rotating shaft 322, and an inner tube 323. The loading platform 321 is located between the first mounting interface 311 and the second mounting interface 312. The loading platform 321 is fixedly connected to the rotating shaft 322 through a flange. A liquid circulation channel is provided inside the loading platform 321. A substrate holder 3211 is provided on the loading platform 321 and is pressed by a pressing plate 3212 fixedly connected to the loading platform 321. The loading platform and the pressing plate can be fixedly connected by screws. The rotating shaft 322 is hollow and is provided with an inner tube 323 communicating with the internal circulation channel of the loading platform. The inner tube divides the cavity of the rotating shaft into a liquid inlet channel and a liquid outlet channel. The liquid inlet channel is communicated with the inlet of the internal liquid circulation channel of the loading platform, and the liquid outlet channel is communicated with the outlet of the internal liquid circulation channel of the loading platform. Liquid inlet 3221 and liquid outlet 3222 respectively connected to the liquid inlet channel and the liquid outlet channel are provided on the rotating shaft. A rotating handwheel 3223 is further provided at the end of the rotating shaft. A magneto-fluid chamber 324 is sleeved outside the rotating shaft; the magneto-fluid chamber is connected to a loading platform interface provided on the oxidation chamber through a flange to achieve high-vacuum sealing of the oxidation chamber. A bearing seat adapted to the rotating shaft is provided on the inner side of the magneto-fluid chamber 341. In this embodiment, liquid nitrogen is used as the coolant. The coolant enters the inner tube 323 through the liquid inlet 3221, enters the loading platform 321 through the inner tube 323, enters the rotating shaft through the internal flow channel of the loading platform 321, and then flows out through the liquid outlet 3222. In order to control the rotation angle of the loading platform, a limit pin 325 is further provided on the loading mechanism 32. The limit pin 325 passes through the rotating handwheel along the direction parallel to the axial direction of the rotating shaft and penetrates into the magneto-fluid chamber 324; the limit pin 325 is threadedly connected to the rotating handwheel 3223 and the magneto-fluid chamber 324. Loosen the limit pin 325, and the angle of the loading platform 321 can be adjusted by rotating the rotating handwheel 3223; tighten the limit pin 325, and the loading platform is positioned.

[0054] A Kaufman ion source 34 is further installed on the oxidation chamber. The sputtering range of the Kaufman ion source 34 covers the loading platform 321.

[0055] A number of heating wires are evenly arranged circumferentially on the inner wall of the oxidation chamber to achieve temperature control inside the oxidation chamber.

[0056] An observation window is provided on the oxidation chamber 31. The observation window faces the loading platform, and the growth, oxidation, and etching conditions of the thin film on the surface of the substrate on the loading platform can be observed.

[0057] As Figure 6As shown in the figure, the on-line thickness monitoring system includes a thickness gauge probe 33, an oscillator 35 connected to the thickness gauge probe 33, a film thickness controller 36 connected to the oscillator 35, and an electron gun power supply 216 and a baffle controller 215 connected to the film thickness controller. The thickness gauge probe 33 is installed on the cover plate 314 at the top of the oxidation chamber 31; the cover plate 314 is detachably connected to the oxidation chamber 31. A quartz crystal is provided on the thickness gauge probe 33, and the quartz crystal and the oscillator form an oscillation circuit; when an electric field is applied to the quartz crystal, an oscillation frequency value can be generated in the oscillation circuit formed by the quartz crystal and the oscillator and sent to the film thickness controller; as the thickness of the coating evaporation material on the quartz crystal is different, the generated frequency value will change. The film thickness controller can obtain the evaporation rate (m (g / s)) of the evaporation raw material based on the change value of the oscillation frequency. The film thickness controller can use a PLC controller.

[0058] (1) When the carrier stage is parallel to the horizontal plane and the middle position of the carrier stage is opposite to the evaporation raw material, the film thickness t0 at the middle position of the carrier stage is:

[0059] t0 = m / 4πρh 2

[0060] In the formula, ρ represents the density of the evaporation raw material, and h represents the distance between the middle position of the carrier stage and the evaporation raw material.

[0061] The film thickness t at a distance x from the middle position of the carrier stage is:

[0062]

[0063] (2) When the carrier stage forms an angle α with the horizontal plane and the middle position of the carrier stage is opposite to the evaporation raw material, the film thickness t′0 at the middle position of the carrier stage is:

[0064] t′0 = t0 cosα

[0065] As Figure 7 shown in the figure, the film thickness t′ at any x (the angle deviating from the middle position is θ) in the direction from the middle position of the carrier stage towards the evaporation raw material is:

[0066]

[0067] The film thickness t″ at any x (the angle deviating from the middle position is θ′) in the direction from the middle position of the carrier stage away from the evaporation raw material is:

[0068]

[0069] Based on the obtained evaporation rate and the density of the evaporation raw material, the thickness distribution of the evaporated film for the sample in normal plating or inclined plating (along the inclination angle of the stage) is calculated according to the above formula. When the thickness distribution of the evaporated film meets the set requirements, the power supply of the electron gun for heating the raw material to be evaporated is controlled to be turned off, and at the same time, the shutter is controlled by the shutter controller to be placed above the evaporation raw material.

[0070] The method for using the above high-vacuum electron beam evaporation thin film deposition equipment is as follows:

[0071] (1) Evaporation coating

[0072] ① Install the sample to be evaporated on the stage;

[0073] ② Close the evaporation chamber and the oxidation chamber, and evacuate the evaporation chamber and the oxidation chamber respectively to meet the vacuum degree requirements;

[0074] ③ Use the Kaufman ion source to etch the surface of the substrate with argon as the gas medium to etch off the oxide layer on the surface of the substrate;

[0075] ④ Evacuate the evaporation chamber and the oxidation chamber again to meet the vacuum degree requirements;

[0076] ⑤ Rotate the stage to the set angle and fix it; and introduce coolant to start the cooling mechanism;

[0077] ⑥ Turn on the electron gun, control the beam current of the electron gun to control the coating rate, and monitor the coating thickness in real time through the on-line thickness monitoring system until the designed film thickness is reached;

[0078] ⑦ Turn off the electron gun.

[0079] (2) Oxidation

[0080] ⑧ Close the gate valve to isolate the evaporation chamber from the oxidation chamber;

[0081] ⑨ Perform dynamic oxidation or static oxidation on the surface of the sample by controlling the oxygen flow rate.

[0082] The above evaporation coating and oxidation processes can be carried out alternately according to the design requirements.

[0083] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, simplifications, and combinations made without departing from the spirit and principle of the present invention shall be equivalent replacement methods and are all included in the protection scope of the present invention.

Claims

1. A high-vacuum electron beam evaporation thin film deposition device, characterized in that, Including: A device support (1), an evaporation device (2) installed on the device support (1), an oxidation device (3) connected to the evaporation device (2) via a gate valve (4), and a vacuum system (5) for evacuating the evaporation device (2) and the oxidation device (3); The above oxidation device (3) includes an oxidation chamber (31) and a carrier mechanism (32) rotatably installed on the oxidation chamber (31); the oxidation chamber (31) is connected to the vacuum system through a pipeline; the oxidation chamber (31) is provided with opposite first mounting interfaces (311) and second mounting interfaces (312); the first mounting interface (311) is connected to the gate valve (4), and the second mounting interface is used for installing a film thickness gauge probe (33); the carrier mechanism (32) includes a carrier table (321) and a rotating shaft (322) fixedly connected to the carrier table; the carrier table (321) is located between the first mounting interface (311) and the second mounting interface (312); a liquid circulation channel is provided inside the carrier table (321), the rotating shaft (322) is hollow and is provided with an inner pipe (323) communicating with the internal circulation channel of the carrier table, and the inner pipe divides the rotating shaft cavity into a liquid inlet channel and a liquid outlet channel; a Kaufman ion source (34) is further installed on the oxidation chamber, and the sputtering range of the Kaufman ion source (34) covers the carrier table (321); the carrier mechanism further includes a magneto-fluid chamber (324) sleeved outside the rotating shaft; the magneto-fluid chamber is connected to a carrier table interface provided on the oxidation chamber through a flange; magneto-fluid is encapsulated in the magneto-fluid chamber; liquid inlet (3221) and liquid outlet (3222) respectively connected to the liquid inlet channel and the liquid outlet channel are provided on the rotating shaft, and a rotating handwheel (3223) is further provided at the end of the rotating shaft; a limit pin (325) is further provided on the carrier mechanism (32), and the limit pin passes through the rotating handwheel along the axial direction of the rotating shaft and penetrates into the magneto-fluid chamber (324); the limit pin (325) is threadedly connected to the rotating handwheel (3223) and the magneto-fluid chamber (324); the oxidation device (3) further includes an on-line thickness monitoring system; The vacuum system (5) includes a first vacuum device (51) for evacuating the evaporation device (2) and a second vacuum device (52) for evacuating the oxidation device (3).

2. The high-vacuum electron beam evaporation thin film deposition equipment according to claim 1, characterized in that, The evaporation device (2) includes a vacuum chamber (21); a first vacuum interface (211) and a third mounting interface (212) are provided on the vacuum chamber (21); the first vacuum device (51) includes a first molecular pump (511) and a first mechanical pump (512); the first molecular pump (511) is connected to the first vacuum interface (211) via a first high-vacuum valve (513); the first mechanical pump (512) is connected to the first vacuum interface (211) and the first molecular pump (511) through pipelines via two low-vacuum valves (514, 515) respectively; the third mounting interface (212) is connected to the gate valve (4).

3. The high-vacuum electron beam evaporation thin film deposition equipment according to claim 1, characterized in that A second vacuum interface (313) is provided on the oxidation chamber (31); the second vacuum device (52) includes a second molecular pump (521) and a second mechanical pump (522); the second molecular pump (521) is connected to the second vacuum interface (313) via a second high-vacuum valve (523); the second mechanical pump (522) is connected to the second vacuum interface (313) and the second molecular pump (521) through pipes via two low-vacuum valves respectively.

4. The high-vacuum electron beam evaporation thin film deposition equipment according to claim 1, characterized in that, One or more gas interfaces are further provided on the oxidation chamber and are connected to corresponding gas supply devices.

5. The high-vacuum electron beam evaporation thin film deposition device according to claim 1, wherein A substrate holder (3211) is provided on the stage (321) and is pressed by a pressing plate (3212) fixedly connected to the stage (321).

6. The high-vacuum electron beam evaporation thin film deposition equipment according to claim 1, characterized in that, A heating device is provided in the oxidation chamber.

7. The high-vacuum electron beam evaporation thin film deposition equipment according to claim 1, characterized in that, The film thickness gauge probe (33) is installed on the cover plate (314) at the top of the oxidation chamber (31); the cover plate (314) is detachably connected to the oxidation chamber (31); the on-line thickness monitoring system includes an oscillator (35) connected to the thickness gauge probe (33), a film thickness controller (36) connected to the oscillator (35), and an electron gun power supply (216) and a baffle controller (215) connected to the film thickness controller.

8. The high-vacuum electron beam evaporation thin film deposition equipment according to claim 1 or 7, characterized in that The evaporation rate m of the evaporation raw material is obtained through the film thickness controller, and then the film layer thickness of the sample on the stage is calculated according to the following formula: (1) When the stage is parallel to the horizontal plane and the middle position of the stage is opposite to the evaporation raw material, the film thickness t0 at the middle position of the stage is: t0 = m / (4πρh) 2 In the formula, ρ represents the density of the evaporation raw material, and h represents the distance between the middle position of the stage and the evaporation raw material; The film thickness t at a distance x from the middle position on the stage is: ; (2) When the stage forms an angle α with the horizontal plane and the middle position of the stage is opposite to the evaporation raw material, the film thickness t′0 at the middle position of the stage is: t′0 = t0cosα The angle of deviation from the middle position at any x in the direction from the middle position of the stage towards the evaporation raw material is θ, and the film thickness t′ at this x is: ; The angle of deviation from the middle position at any x in the direction away from the evaporation raw material from the middle position of the stage is θ′, and the film thickness t″ at this x is:

Citation Information

Patent Citations

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