Magnetron sputtering coating device and coating method

Abstract

The invention relates to a magnetron sputtering coating device and a coating method. The magnetron sputtering coating device comprises a reaction chamber, a magnetron target, an ion source and a sample table, the reaction chamber is of a vacuum sealing structure; the magnetic control target is fixed and communicated with the bottom surface of the reaction chamber; the ion source comprises a first ion source and a second ion source which are symmetrically arranged, and the first ion source and the second ion source are respectively fixed and communicated with the side surfaces of the two ends of the reaction chamber; the ion source comprises a first gas inlet, a transmission channel and an outlet, and the first gas inlet is used for introducing reaction gas into the ion source from the outside of the reaction chamber; and the sample table is positioned at the top end of the reaction chamber. According to the method, the symmetrical double-ion-source ionization reaction gas is matched with sputtering of the magnetron target, and the film is coated on the substrate in a reaction manner, so that the ionization rate of the gas is increased, the target poisoning phenomenon during sputtering is inhibited, the film coating rate is increased, and the preparation of the single-crystal or polycrystalline film at the low temperature is realized.

Description

Technical Field

[0001] The present invention relates to the technical field of film coating devices, and in particular to a magnetron sputtering film coating device and a film coating method. Background Art

[0002] Magnetron sputtering coating technology is an advanced coating technology used to deposit single-layer / multi-layer thin film materials on the surface of a substrate. This technology has the advantages of fast film deposition rate, wide applicability, good film uniformity, strong adhesion and applicability to various materials, and is widely used in electronics, optics, energy, protection and other fields.

[0003] In recent years, magnetron sputtering technology has developed towards a more efficient and diversified direction. For example, the prior art CN113913737A discloses a method for preparing a nanoporous double-layer thin film material, firstly using magnetron sputtering technology to deposit a TiAlN film on an Al2O3 substrate, then magnetron sputtering to deposit a NiCr-Ti precursor film thereon, and then etching with a hydrofluoric acid solution to finally form a porous NiCr / TiAlN alloy thin film coating material. The double-layer thin film prepared by this preparation method has a complete and continuous porous structure, uniform shape, controllable size, and strong interface adhesion between layers.

[0004] Existing magnetron sputtering mainly includes direct magnetron sputtering and reactive magnetron sputtering. The principle of direct magnetron sputtering is that a direct current power supply (DC) or a radio frequency power supply (RF) is directly connected to a magnetron target (metal target, alloy target or compound target), and the working gas is ionized and accelerated under the action of the electric field and hits the surface of the target material, so that the target atoms are sputtered and deposited on the surface of the substrate. The principle of reactive magnetron sputtering means that in reactive magnetron sputtering, reactive gases such as nitrogen or oxygen are introduced into the vacuum chamber. This gas is ionized and reacted due to high-energy collisions in the plasma environment. When the sputtered metal atoms on the target reach the substrate, they react with the reactive gas to form compounds and deposit on the surface of the substrate.

[0005] However, direct magnetron sputtering has the disadvantages of slow deposition rate in depositing compounds, especially oxide and nitride films, and the deposited films are mostly amorphous films, and the preparation of crystalline films can only be achieved at a higher substrate temperature. Traditional reactive magnetron sputtering directly introduces working gas and reactive gas into the reaction vacuum chamber. The deposition process has the disadvantages of low reactive gas ionization rate, easy target poisoning, low reaction rate between reactive gas and sputtering target atoms, and difficulty in obtaining compound films with ideal stoichiometric ratios.

[0006] Therefore, how to increase the deposition rate of magnetron sputtering coating equipment and improve the ionization of the reaction gas by the equipment, while effectively suppressing target poisoning and obtaining a crystal film with an ideal stoichiometric ratio has become a problem that needs to be solved urgently. Summary of the invention

[0007] In order to solve the above technical problems, the purpose of the present invention is to provide a magnetron sputtering coating device and coating method. The present invention directly ionizes the reaction gas through a symmetrically arranged dual ion source and cooperates with the sputtering of the magnetron target arranged at the bottom of the device to perform reaction coating on the substrate at the sample stage at the top of the device, thereby improving the ionization rate of the reaction gas, suppressing the target poisoning phenomenon during sputtering, and the ionized gas directly reacts with the sputtered target material, thereby improving the reaction rate and coating rate, and successfully realizing the preparation of single crystal or polycrystalline thin films with ideal stoichiometric ratio at low temperature.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides a magnetron sputtering coating device, the magnetron sputtering coating device comprising a reaction chamber, a magnetron target, an ion source and a sample stage;

[0010] The reaction chamber is a vacuum sealing structure;

[0011] The magnetron target is fixed and connected to the bottom surface of the reaction chamber;

[0012] The ion source comprises a first ion source and a second ion source which are symmetrically arranged, wherein the first ion source and the second ion source are respectively fixed and connected to the two end sides of the reaction chamber; the ion source comprises a first gas inlet, a transmission channel and an outlet, wherein the first gas inlet is used to introduce a reaction gas from the outside of the reaction chamber into the ion source;

[0013] The sample stage is located at the top of the reaction chamber.

[0014] In the magnetron sputtering coating device provided by the present invention, symmetrical dual ion sources are arranged on the two end sides of the reaction chamber, and an air inlet is arranged on the ion source, so that the reaction gas directly enters the ion source through the air inlet arranged on the ion source, and the reaction gas is directly ionized into plasma in the ion source, and under the action of the electric field, the plasma beam is drawn out and shot toward the sample stage, so that the successful ionization of the reaction gas is achieved, and the ionization rate of the reaction gas is improved. More importantly, the reaction gas is directly introduced into the ion source, which can also effectively suppress the target poisoning phenomenon. The symmetrical arrangement of the first ion source and the second ion source can further increase the content of the ionized gas, thereby making the deposition rate of the device faster.

[0015] The present invention sets a sample stage at the top of a reaction chamber, sets a magnetron target at the bottom of the reaction chamber, and sets a dual ion source symmetrically at both ends of the reaction chamber. The dual ion sources symmetrically set at both ends of the device are used to ionize the reaction gas and sputter the target material of the magnetron target at the bottom of the device, so that the substrate on the sample stage set at the top of the device can be plated together. The target atoms sputtered by the magnetron target directly react with the plasma state of the reaction gas ionized by the ion source flow, which can improve the reaction efficiency and rate between the plasma beam of the ionized reaction gas and the sputtered target atoms. In addition, the reaction gas is directly introduced into the ion source for ionization, which can significantly improve the ionization content of the reaction gas and effectively suppress the target poisoning phenomenon in the reaction sputtering process, thereby improving the deposition rate of the coating device.

[0016] Preferably, fixing components are provided on the side surfaces at both ends of the reaction chamber for fixing the ion source.

[0017] Preferably, with the direction of the sample placement plane of the sample stage as the horizontal direction, the placement directions of the first ion source and the second ion source are both 30-60° to the horizontal direction of the sample stage, for example, 30°, 35°, 40°, 45°, 50°, 55° or 60°.

[0018] The present invention sets the placement direction of the ion source so that it forms a fixed angle with the direction of the sample placement plane of the sample stage, which can further increase the contact area between the plasma beam after the reaction gas is ionized and the sample stage, thereby increasing the reaction efficiency and reaction probability between the reaction gas ion beam and the target material atoms sputtered by the magnetron target. In the present invention, if the placement direction of the ion source is too small with the horizontal direction of the sample stage, most of the ionized reaction gas plasma will be ejected toward the reaction chamber, while the content of plasma that is ejected toward and reaches the sample stage to participate in the reaction will be relatively small; if the angle is too large, the reaction gas plasma beam ionized by the ion source will be directly ejected toward the sample stage, causing the reaction gas ion beam to etch the thin film deposited on the substrate, resulting in a porous surface of the thin film, thereby reducing the quality of the thin film.

[0019] Preferably, the first ion source and the second ion source are at the same distance from the center of the sample stage.

[0020] Preferably, the ion source comprises an annular structure.

[0021] The annular structure ion source of the present invention has a more uniform internal magnetic control distribution, thereby being able to ionize a more uniform plasma.

[0022] Preferably, the ion source comprises an anode layer ion source.

[0023] The present invention adopts an anode layer ion source, which has the advantages of high gas ionization rate, simple structure and easy maintenance.

[0024] Preferably, the ion source further comprises an electromagnetic shielding cover.

[0025] The electromagnetic shielding cover in the present invention is made of magnetically conductive alloy, including but not limited to 1Cr17 stainless steel.

[0026] Preferably, the electromagnetic shielding cover is a hollow annular structure.

[0027] Preferably, a connecting shaft is provided in the central area of ​​the bottom surface of the electromagnetic shielding cover, and the connecting shaft is fixed to and communicated with the bottom surface of the electromagnetic shielding cover and extends to the outside of the bottom surface.

[0028] In the present invention, a part of the connecting shaft is located inside the electromagnetic shielding cover, and a part of the connecting shaft is located outside the electromagnetic shielding cover.

[0029] Preferably, in the magnetron sputtering coating device, the connecting shaft extending to the outside of the electromagnetic shielding cover of the ion source is connected to the fixing parts arranged on the two end sides of the reaction chamber, so as to fix the ion source and connect it to the two end sides of the reaction chamber.

[0030] Preferably, a first monopole magnet hollow column is also arranged on the inner bottom surface of the electromagnetic shielding cover, and a second monopole magnet hollow column is arranged on the upper end of the first monopole magnet hollow column, and the first monopole magnet hollow column and the second monopole magnet hollow column both surround and are fixed to the side of the connecting shaft.

[0031] Preferably, the first monopole magnet hollow column and the second monopole magnet hollow column are both fixed to the connecting shaft via a connecting rod.

[0032] In the present invention, the connecting shaft may be a flange connecting component; the connecting rod used to fix the first monopole magnet hollow column and the second monopole magnet hollow column on the connecting shaft may be a screw rod.

[0033] Preferably, the first monopole magnet hollow column and the second monopole magnet hollow column are both hollow annular structures.

[0034] In the ion source of the present invention, the function of the first monopole magnet hollow column is to form a monopole magnetic field; the function of the second monopole magnet hollow column is to form a monopole magnetic field. The polarities of the first monopole magnet and the second monopole magnet are opposite, and a closed magnetic field is formed inside the ion source through the cooperation of the first and second monopole magnets.

[0035] Preferably, an inner anode ring is arranged on the outer side of the second monopole magnet hollow column away from the connecting shaft.

[0036] Preferably, the inner anode ring is fixed to the inside of the electromagnetic shielding cover via supporting connecting rods.

[0037] Preferably, there is a spacing area between the inner anode ring and the second monopole magnet hollow column for ionizing the reaction gas.

[0038] Optionally, the width of the spacing area is 0.5-1.0 cm, such as 0.5 cm, 0.6 cm, 0.7 cm, 0.8 cm, 0.9 cm or 1.0 cm, etc.

[0039] Preferably, the opening of the opening gap between the upper end of the electromagnetic shielding cover and the second monopole magnet hollow column is the outlet of the ion source.

[0040] Preferably, the spaced area inside the electromagnetic shield is a transmission channel of the ion source.

[0041] Preferably, the first monopole magnet hollow column, the second monopole magnet hollow column and the inner anode ring are all arranged inside the electromagnetic shielding cover.

[0042] Preferably, a water cooling groove is further provided inside the electromagnetic shielding cover, and the water cooling groove is located on the outer side of the hollow column of the first monopole magnet away from the connecting shaft.

[0043] In the present invention, a water cooling tank is provided in the electromagnetic shielding cover of the ion source in order to cool the monopole magnet and prevent the monopole magnet from being demagnetized due to overheating during operation, which eventually causes the ion source to fail to work.

[0044] Preferably, the water cooling groove is a hollow annular channel structure.

[0045] Preferably, the water cooling groove surrounds the side surface of the first monopole magnet hollow column.

[0046] The present invention further adopts a water cooling groove with a hollow annular channel structure in order to increase the contact area with the annular magnet and further enhance the cooling effect.

[0047] Preferably, a water cooling inlet and a water cooling outlet are also provided at the bottom of the water cooling tank.

[0048] Preferably, the lower ends of the water cooling inlet and the water cooling outlet extend outward to the outside of the bottom surface of the electromagnetic shielding cover and are connected to the bottom surface of the electromagnetic shielding cover.

[0049] Preferably, the water cooling inlet and the water cooling outlet are respectively located on two sides of the first monopole magnet hollow column.

[0050] Preferably, the first air inlet in the ion source is connected to the bottom surface of the electromagnetic shielding cover and extends to the outside of the bottom surface.

[0051] The present invention sets a first air inlet in the ion source, which is connected to the bottom surface of the electromagnetic shielding cover and extends to the outside of the bottom surface. The reaction gas outside the coating device can be directly introduced into the ion source for ionization reaction, thereby effectively improving the ionization content of the reaction gas by the ion source, and can also effectively suppress target poisoning during the reactive sputtering process.

[0052] Preferably, the ion source further comprises a power supply interface, the upper end of which is connected to the inner anode ring, and the lower end of which is connected to the bottom surface of the electromagnetic shielding cover and extends to the outside of the bottom surface.

[0053] Preferably, the first monopole magnet hollow column, the second monopole magnet hollow column, the inner anode ring and the water cooling tank in the ion source are all located inside the reaction chamber.

[0054] Preferably, the first air inlet provided on the bottom surface of the electromagnetic shielding cover is located outside the reaction chamber.

[0055] Preferably, the water cooling inlet and the water cooling outlet arranged on the bottom surface of the electromagnetic shielding cover are both located outside the reaction chamber.

[0056] Preferably, the power interface of the electromagnetic shielding cover arranged outside the bottom surface is located outside the reaction chamber.

[0057] Preferably, the magnetron sputtering coating device further comprises an ion source power supply and a magnetron target power supply located outside the reaction chamber.

[0058] Preferably, the number of the ion source power supplies is the same as the number of the ion sources.

[0059] Preferably, the number of the magnetron target power supplies is the same as the number of the magnetron targets.

[0060] In the present invention, there is no specific limitation on the number of magnetron targets, including but not limited to 1, 2 or 3, etc., and those skilled in the art can select according to needs.

[0061] Preferably, the ion source power supply is connected to a power supply interface in the ion source.

[0062] Preferably, the magnetron target power supply is connected to the magnetron target.

[0063] Preferably, the magnetron target power supply includes any one of a high power pulse power supply (HiPIMS power supply), a radio frequency power supply or a direct current power supply, or a combination of at least two of them.

[0064] Preferably, the magnetron target power supply is a high-power pulse power supply.

[0065] In the present invention, the "high-power pulse power supply" used refers to a power supply with a peak current greater than or equal to 1A, a power greater than or equal to 2000W, a pulse frequency greater than or equal to 1000Hz, and a duty cycle adjustable between 10-90%.

[0066] The magnetron target power supply of the present invention adopts a specific power supply, which can increase the rate at which the magnetron target material is sputtered into target material atoms, thereby increasing the sputtering rate of the magnetron sputtering coating device. It is further preferred that a high-power pulse magnetron target power supply cooperates with a symmetrically arranged dual ion source to accelerate the coating speed of the device.

[0067] Preferably, the reaction chamber is provided with a second gas inlet for introducing working gas into the reaction chamber.

[0068] The present invention sets a second air inlet in the reaction chamber to introduce working gas. The working gas enters the reaction chamber and can be ionized into plasma. Under the action of the electric field, the plasma bombards the target material on the magnetron target, sputters out target material atoms, and the target material atoms react with the plasma beam ionized and ejected from the ion source to quickly form a film and deposit on the substrate surface. The present invention uses the first air inlet set on the ion source to directly pass the reaction gas into the ion source, and uses the second air inlet set on the reaction chamber to pass the working gas into the reaction chamber. Through the separate design of the reaction gas inlet and the working gas inlet, target poisoning in the reactive sputtering process can be effectively avoided.

[0069] Preferably, the magnetron sputtering coating device further comprises a servo motor located outside the top surface of the reaction chamber.

[0070] Preferably, a connecting rod is provided on the sample stage.

[0071] Preferably, the servo motor passes through the top surface of the reaction chamber through a connecting channel to be connected to a connecting rod on the sample stage, so as to drive the rotation of the sample stage.

[0072] The present invention introduces a servo motor to drive the rotation of the sample stage, which can make the coating of the device more uniform.

[0073] Preferably, the connecting channel in the servo motor and the connecting rod on the sample stage are transmitted via a transmission element.

[0074] Preferably, the sample stage is a hollow frame structure.

[0075] The present invention adopts a sample stage with a hollow frame structure, which can be compatible with sample substrates of 4 inches or less in size.

[0076] Preferably, the magnetron sputtering coating device further comprises a vacuum gauge arranged outside the reaction chamber for measuring the vacuum degree in the reaction chamber.

[0077] Preferably, the vacuum gauge is connected to the interior of the reaction chamber via a connecting component.

[0078] Preferably, the connecting component comprises a hollow flange.

[0079] Preferably, the magnetron sputtering coating device further comprises an observation window arranged on a side of the reaction chamber for observing the sputtering process.

[0080] Preferably, the observation window is not on the same side as the first ion source and the second ion source.

[0081] Preferably, the magnetron sputtering coating device further comprises a pump group, a flow limiting valve and a gas mass flow meter, which are used to obtain and regulate the vacuum degree of the reaction chamber.

[0082] In the present invention, a pump group is used to evacuate the reaction chamber to obtain the background vacuum of the reaction chamber, and a flow limiting valve and a gas mass flow meter are used to control the flow of the working gas entering the reaction chamber and the working vacuum of the reaction chamber.

[0083] Preferably, the pump group, the flow limiting valve and the gas mass flow meter are located outside the reaction chamber.

[0084] Preferably, the pump group, the flow limiting valve and the gas mass flow meter are all connected to the interior of the reaction chamber through a connecting component.

[0085] Preferably, the connection component connecting the pump group, the flow limiting valve and the gas mass flow meter comprises a flange.

[0086] Preferably, the pump group includes a front-stage mechanical pump and / or a molecular pump.

[0087] In a second aspect, the present invention provides a magnetron sputtering coating method based on the magnetron sputtering coating device described in the first aspect, and the specific process of the magnetron sputtering coating method includes:

[0088] A substrate is placed on a sample stage, and a reaction chamber is evacuated; reaction gases are introduced into the two ion sources from the first air inlets of the symmetrically arranged first ion source and the second ion source, respectively, and circulated through the transmission channel. In the two ion sources, the reaction gases are ionized into plasma to form a plasma beam, and then reach the outlets of the two ion sources through the transmission channel, and are ejected onto the substrate under the action of an electric field; at the same time, a magnetron target material in the magnetron target is sputtered into target material atoms; the target material atoms react with the plasma beam ejected onto the substrate, and a thin film is deposited and prepared on the substrate.

[0089] The magnetron sputtering coating method provided by the present invention is based on a specifically designed magnetron sputtering coating device, and adopts the first air inlets on the symmetrically arranged first ion source and the second ion source to directly pass the reaction gas into the ion source for ionization, thereby improving the ionization content and ionization efficiency of the reaction gas and effectively avoiding the occurrence of target poisoning. The formed plasma beam and the target material atoms sputtered by the magnetron target material in the magnetron target directly react to form a film on the substrate located on the sample stage, which not only improves the deposition rate but also can directly plate single crystal / polycrystalline thin films on the surface of the substrate at low temperature.

[0090] Preferably, the thin film prepared on the base substrate is any one of a single crystal thin film and a polycrystalline thin film.

[0091] The magnetron sputtering coating device of the present invention can achieve efficient ionization of the reaction gas, thereby improving the reaction efficiency and rate with the sputtered target atoms, and because the film is formed by direct reaction on the surface of the substrate, it further achieves the successful preparation of single crystal or polycrystalline thin films at low temperatures.

[0092] Preferably, the reaction gas includes any one of Ar, O2, N2, NH3 or C2H4, or a combination of at least two of them.

[0093] The ion source provided by the present invention can realize the ionization of various reaction gases, thereby expanding the application scope of the magnetron sputtering coating device.

[0094] Preferably, the magnetron target material includes any one of Al, Y, Sc, Fe, Ta, Si or Ti, or a combination of at least two of them.

[0095] Preferably, during the vacuuming process, a pump group is used to evacuate the reaction chamber until the background vacuum degree of the reaction chamber is 8×10 -5 Pa or less, for example 8×10 -5 Pa, 7×10 -5 Pa, 6×10 -5 Pa, 5×10 -5 Pa, 4×10 -5 Pa, 3×10 -5 Pa, 2×10 -5 Pa or 1×10 -5 Pa et al.

[0096] Preferably, after the vacuuming, the magnetron sputtering coating method also includes introducing a working gas into the reaction chamber, and adjusting the working vacuum degree in the reaction chamber to 0.5-1.5Pa, such as 0.5Pa, 0.7Pa, 0.9Pa, 1.1Pa, 1.3Pa or 1.5Pa, etc., by using a gas mass flow meter and a limiting valve.

[0097] Preferably, before the reaction gas is introduced into the ion source, the method further comprises turning on an ion source power supply connected to the ion source and a magnetron target power supply connected to the magnetron target respectively.

[0098] Preferably, during the ionization process, the current of the first ion source and the second ion source is set to 50-300 mA, such as 50 mA, 100 mA, 150 mA, 200 mA, 250 mA or 300 mA.

[0099] Preferably, during the ionization process, the flow rate of the reaction gas is 5-60sccm, for example, 5sccm, 10sccm, 15sccm, 20sccm, 25sccm, 30sccm, 35sccm, 40sccm, 45sccm, 50sccm, 55sccm or 60sccm, etc.

[0100] Preferably, during the ionization process of the reaction gas, cooling water is introduced into the water cooling tank through the water cooling inlet and then flows out from the water cooling outlet.

[0101] Preferably, during the ionization process of the reaction gas, a first monopole magnet hollow column and a second monopole magnet hollow column are used to form a closed magnetic field, and the reaction gas is ionized into plasma under the action of the magnetic field and the inner anode ring.

[0102] Preferably, the specific process of sputtering the magnetron target material into target material atoms includes: introducing a working gas into the reaction chamber through a second gas inlet provided in the reaction chamber, and ionizing the working gas into plasma through an electric field between the magnetron target and the reaction chamber, and the plasma is accelerated under the action of the electric field and collides with the surface of the magnetron target material in the magnetron target, thereby sputtering out the target material atoms.

[0103] Preferably, the working gas comprises an inert gas.

[0104] Preferably, during the sputtering of the magnetron target into target atoms, the power of the magnetron target is set to 100-400W, such as 100W, 150W, 200W, 250W, 300W, 350W or 400W.

[0105] Preferably, during the sputtering of the magnetron target into the target atoms, a gas mass flow meter is used to set the flow rate of the working gas to 5-30 sccm, for example, 5 sccm, 10 sccm, 15 sccm, 20 sccm, 25 sccm or 30 sccm.

[0106] Preferably, the ratio of the flow rate of the working gas to the flow rate of the reaction gas is 1:(1-3), such as 1:1, 1:1.5, 1:2, 1:2.5 or 1:3.

[0107] In the present invention, the ratio of the working gas flow rate to the reaction gas flow rate is regulated in order to regulate the atomic stoichiometric ratio of the obtained compound film. The magnetron sputtering coating method of the present invention adopts a specific magnetron sputtering coating device, which can accurately regulate the atomic stoichiometric ratio of the compound of the film by regulating the ratio of the working gas flow rate to the reaction gas flow rate.

[0108] Compared with the prior art, the present invention has at least the following beneficial effects:

[0109] (1) The magnetron sputtering coating device provided by the present invention sets the sample stage at the top of the reaction chamber, sets the magnetron target at the bottom of the reaction chamber, and sets symmetrical dual ion sources at both ends of the reaction chamber. The dual ion sources symmetrically set at both ends of the device are used to ionize the reaction gas and cooperate with the target material sputtering of the magnetron target at the bottom of the device to perform reactive sputtering film formation on the substrate on the top sample stage. The target material atoms sputtered by the magnetron target directly react with the ionized plasma state of the reaction gas ejected by the ion source flow, thereby improving the reaction efficiency and rate between the plasma beam of the ionized reaction gas and the sputtered target material atoms. In addition, the reaction gas is directly introduced into the ion source for ionization, which can significantly improve the ionization content of the reaction gas and effectively suppress target poisoning during the reactive sputtering process, thereby improving the reactive sputtering rate of the coating device.

[0110] (2) The magnetron sputtering coating method provided by the present invention is based on a specifically designed magnetron sputtering coating device, and adopts the first air inlet on the symmetrically arranged first ion source and the second ion source to directly introduce the reaction gas into the ion source for ionization, thereby improving the ionization content and ionization efficiency of the reaction gas and effectively avoiding the occurrence of target poisoning. The formed plasma beam and the target material atoms sputtered by the magnetron target material in the magnetron target directly react to form a film on the substrate located on the sample stage, which not only improves the deposition rate but also can directly coat single crystal / polycrystalline thin films on the surface of the substrate at low temperature. BRIEF DESCRIPTION OF THE DRAWINGS

[0111] Figure 1 It is a schematic diagram of the main structure of the magnetron sputtering coating device provided in Example 1 of the present invention.

[0112] Figure 2 It is a left-side structural schematic diagram of the magnetron sputtering coating device provided in Example 1 of the present invention.

[0113] Among them, 1, reaction chamber; 1-1, second air inlet; 1-2, ion source fixing component; 2, magnetron target; 3, ion source; 4, sample stage; 5, servo motor; 6, vacuum gauge; 7, observation window; 8, pump group; 9, flow limiting valve; 10, gas mass flow meter; 11, ion source power supply; 12, magnetron target power supply.

[0114] Figure 3 It is a top view schematic diagram of the arrangement of the magnetron targets in the magnetron sputtering coating device provided in Example 1 of the present invention on the bottom surface of the reaction chamber.

[0115] Figure 4 It is a cross-sectional schematic diagram of the main view of the first ion source and the second ion source in the magnetron sputtering coating device provided in Example 1 of the present invention.

[0116] Among them, 3-1, electromagnetic shielding cover; 3-2, first air inlet; 3-3, power interface; 3-4, outlet; 3-5, transmission channel; 3-6, connecting shaft; 3-7, first monopole magnet hollow column; 3-8, second monopole magnet hollow column; 3-9, inner anode ring; 3-10, water cooling groove; 3-11, water cooling inlet; 3-12, water cooling outlet.

[0117] Figure 5 This is the X-ray diffraction pattern (XRD pattern) of the aluminum nitride film prepared in Example 1 of the present invention.

[0118] Figure 6 This is the X-ray diffraction pattern (XRD pattern) of the film prepared in Example 10 of the present invention.

[0119] Figure 7 It is the X-ray diffraction pattern (XRD pattern) of the film prepared in Comparative Example 2 of the present invention. DETAILED DESCRIPTION

[0120] The technical solution of the present invention is further described below in conjunction with the accompanying drawings and through specific implementation methods. However, the following examples are only simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention shall be subject to the claims.

[0121] The parameters of the high-power pulsed DC power supply used in the following embodiments are: peak current of 1A, duty cycle of 50%, frequency of 1000Hz, and power of 2000W.

[0122] Example 1

[0123] This embodiment provides a magnetron sputtering coating device, and its main structural diagram is as follows: Figure 1 As shown, the left view structure diagram is as follows Figure 2As shown, it specifically includes a reaction chamber 1, a magnetron target 2, an ion source 3, a sample stage 4, a servo motor 5, a vacuum gauge 6, an observation window 7, a pump group 8, a flow limiting valve 9, a gas mass flow meter 10, an ion source power supply 11 and a magnetron target power supply 12.

[0124] The reaction chamber 1 is a vacuum sealed structure. A second air inlet 1-1 is provided on the reaction chamber 1 for introducing working gas. Two ion source fixing components 1-2 are symmetrically provided at both ends of the reaction chamber 1 for fixing the ion source 3.

[0125] The magnetron target 2 is fixed and connected to the bottom surface of the reaction chamber 1, and the lower end is connected to a magnetron target power supply 12, which adopts a high-power pulsed DC power supply. The interior of the magnetron target 2 also contains a magnetron target material. Three magnetron targets 2 are arranged on the bottom surface of the reaction chamber 1, which are respectively denoted as target A, target B and target C. The top view schematic diagram of the arrangement of the magnetron targets on the bottom surface of the reaction chamber 1 is shown in FIG. Figure 3 described.

[0126] The ion source 3 includes a first ion source and a second ion source which are symmetrically arranged. The first ion source and the second ion source are respectively fixed by ion source fixing parts 1-2 and connected to the two end sides of the reaction chamber 1. The direction of the sample placement plane of the sample stage 4 is taken as the horizontal direction. The placement directions of the first ion source and the second ion source are both 45° to the horizontal direction of the sample stage 4. The centers of the outlets 3-4 of the first ion source and the second ion source are the same from the center of the sample stage 4. The components and structures of the first ion source and the second ion source are the same, and both are anode layer ion sources of annular structures. The cross-sectional diagrams in the main views of the first ion source and the second ion source are as shown in FIG. Figure 4 As shown, the specific configuration is as follows:

[0127] The first ion source and the second ion source are both provided with a hollow annular electromagnetic shielding cover 3-1 made of 1Cr17 stainless steel, the bottom opening of which is provided with a first air inlet 3-2 and a power interface 3-3, an outlet 3-4 is provided at the upper opening, and the internal spacing area serves as a transmission channel 3-5. The first air inlet 3-2 is connected to the bottom surface of the electromagnetic shielding cover 3-1 and extends to the outside of the bottom surface, and is used to introduce reaction gas from the outside of the reaction chamber into the ion source. The lower end of the power interface 3-3 is connected to the bottom surface of the electromagnetic shielding cover 3-1 and extends to the outside of the bottom surface to be connected to the ion source power supply 12. There are two ion source power supplies 11, which are respectively connected to the lower ends of the power interfaces 3-3 in the first ion source and the second ion source.

[0128] A connecting shaft 3-6 is arranged in the central area of ​​the bottom surface of the electromagnetic shielding cover 3-1. The connecting shaft 3-6 is a flange connecting component. The connecting shaft 3-6 is fixed and connected to the bottom surface of the electromagnetic shielding cover 3-1 and extends to the outside of the bottom surface. One section of the connecting shaft 3-6 is located inside the electromagnetic shielding cover 3-1, and one section of the connecting shaft 3-6 is located outside the electromagnetic shielding cover 3-1. The connecting shaft 3-6 extending to the outside of the electromagnetic shielding cover 3-1 of the ion source 3 is connected to the ion source fixing component 1-2 arranged on the two end sides of the reaction chamber 1.

[0129] In the first ion source and the second ion source, the inner bottom surface of the electromagnetic shielding cover 3-1 is also provided with a first monopole magnet hollow column 3-7 with a hollow ring structure, and a second monopole magnet hollow column 3-8 with a hollow ring structure is provided at the upper end of the first monopole magnet hollow column 3-7. The first monopole magnet hollow column 3-7 and the second monopole magnet hollow column 3-8 are both surrounded by and fixed on the side of the connecting shaft 3-6, and are fixed to the connecting shaft 3-6 set by a flange connection component through screw rods arranged on the inner sides of the first monopole magnet hollow column 3-7 and the second monopole magnet hollow column 3-8. The first monopole magnet hollow column 3-7 is an S-pole magnet, and the second monopole magnet hollow column 3-8 is an N-pole magnet. An inner anode ring 3-9 is arranged on the outer side of the second monopole magnet hollow column 3-8 away from the connecting shaft 3-1, and there is a spacing area between the inner anode ring 3-9 and the second monopole magnet hollow column 3-8 for ionizing the reaction gas, and the width of the spacing is 1.0 cm. The inner anode ring 3-9 is fixed to the inside of the electromagnetic shielding cover 3-1 by a supporting connecting rod, and the lower end of the inner anode ring 3-9 is connected to the upper end of the power interface 3-3. The first monopole magnet hollow column 3-7, the second monopole magnet hollow column 3-8 and the inner anode ring 3-9 are all arranged inside the electromagnetic shielding cover 3-1, and the opening of the open gap between the upper end of the electromagnetic shielding cover 3-1 and the second monopole magnet hollow column 3-8 serves as the outlet 3-4 of the ion source 3.

[0130] The interior of the electromagnetic shielding cover 3-1 is also provided with a water cooling groove 3-10 of a hollow annular channel structure. The water cooling groove 3-10 is located on the outer side of the first monopole magnet hollow column 3-7 away from the connecting shaft 3-6. The water cooling groove 3-10 surrounds the side of the first monopole magnet hollow column 3-7. Water cooling inlet 3-11 and water cooling outlet 3-12 are also provided on both sides of the bottom of the water cooling groove 3-10. The lower ends of the water cooling inlet 3-11 and the water cooling outlet 3-12 extend outward to the outside of the bottom surface of the electromagnetic shielding cover 3-1 and are connected to the bottom surface of the electromagnetic shielding cover 3-1. The water cooling inlet 3-11 and the water cooling outlet 3-12 are respectively located on both sides of the first monopole magnet hollow column 3-7.

[0131] A connecting shaft 3-4 extending to the outside of the electromagnetic shielding cover 3-1 of the ion source 3 is connected to the ion source fixing parts 1-2 symmetrically arranged on the two end sides of the reaction chamber 1, and the first ion source and the second ion source are respectively fixed and connected to the two end sides of the reaction chamber 1. The outlets 3-4, the transmission channel 3-5, the first monopole magnet hollow column 3-7, the second monopole magnet hollow column 3-8, the inner anode ring 3-9, the water cooling groove 3-10 in the first ion source and the second ion source, part of the connecting shaft 3-6 and part of the power interface 3-3 are all located inside the reaction chamber 1. The first air inlet 3-2, the water cooling inlet 3-11, the water cooling outlet 3-12, the lower end of the power interface 3-3 and the lower end of the connecting shaft 3-6 arranged on the bottom surface of the electromagnetic shielding cover 3-1 of the ion source 3 all extend to the outside of the reaction chamber 1.

[0132] The sample stage 4 of the magnetron sputtering coating device is arranged at the top of the reaction chamber 1. The sample stage 4 adopts a hollow frame structure capable of supporting the substrate material, and is made of 304 stainless steel. The servo motor 5 outside the top surface of the reaction chamber 1 passes through the top surface of the reaction chamber 1 through a connecting channel to be connected to the connecting rod on the sample stage 4, and is used to drive the sample stage 4 to rotate. The connecting channel adopts a flange connecting channel, and the connecting rod is a mechanical connecting rod. The flange connecting channel in the servo motor 5 and the mechanical connecting rod on the sample stage 4 are driven by a belt as a transmission element.

[0133] The vacuum gauge 6 is disposed outside the reaction chamber 1 and is connected to the inside of the reaction chamber 1 through a hollow flange, and is used to measure the vacuum degree in the reaction chamber 1 .

[0134] The observation window 7 is disposed on the side of the reaction chamber 1 for observing the sputtering process. The observation window 7 and the first ion source and the second ion source are not on the same side of the reaction chamber 1 .

[0135] The pump group 8, the flow limiting valve 9 and the gas mass flow meter 10 are located outside the reaction chamber 1, and are connected to the interior of the reaction chamber 1 through a flange. The pump group 8, the flow limiting valve 9 and the gas mass flow meter 10 are used to obtain and regulate the vacuum degree of the reaction chamber 1. The pump group 8 is composed of a front-stage mechanical pump and a molecular pump.

[0136] The present invention provides a magnetron sputtering coating method based on the above magnetron sputtering coating device, and the specific steps are as follows:

[0137] (1) A (100) oriented single crystal silicon wafer was used as a substrate. The single crystal silicon wafer was immersed in a 10 wt% hydrofluoric acid solution for 60 s, then ultrasonically cleaned in acetone for 20 min, then rinsed with ultrapure water, and finally dried with nitrogen to obtain a cleaned substrate.

[0138] (2) Place the cleaned silicon substrate on the hollow frame of the sample stage, and use the front-stage mechanical pump and molecular pump to evacuate the reaction chamber until the background vacuum of the reaction chamber measured by the vacuum gauge is 8×10 - 5 Pa, turn on the gas mass flow meter, set the working flow rate of the working gas argon to 10 sccm, then adjust the opening of the limiting valve, and use the gas mass flow meter and the limiting valve to adjust the working vacuum degree in the reaction chamber to 1 Pa.

[0139] (3) Turn on the ion source power supply, set the current of the first ion source and the second ion source to 100 mA, use the water-cooling inlet to continuously introduce cooling water into the hollow annular water-cooling groove, and then flow out from the water-cooling outlet. Use nitrogen as the reaction gas, set the nitrogen flow rate to 30 sccm, and allow the nitrogen to enter the two ion sources from the first air inlet in the symmetrically arranged first ion source and the second ion source, respectively, and flow through the transmission channel. In the first ion source and the second ion source, a closed magnetic field is formed by the first monopole magnet hollow column and the second monopole magnet hollow column. Under the action of the magnetic field and the inner anode ring, the nitrogen is ionized into plasma to form a plasma beam, and then reaches the outlets of the first ion source and the second ion source through the transmission channel, and is ejected onto the substrate of the sample stage under the action of the electric field.

[0140] While turning on the ion source power supply, turn on the magnetron target power supply of the high-power pulsed DC power supply, and use aluminum metal with a size of 3 inches and a purity of 99.99% as the magnetron target material. It is located in the three magnetron targets set on the bottom of the reaction chamber. The magnetron target power is set to 200W, and argon continues to enter the reaction chamber through the second gas inlet set in the reaction chamber. The flow rate of argon is maintained at 10sccm. The argon is ionized into plasma through the electric field between the magnetron target and the reaction chamber. The ionized plasma is accelerated under the action of the electric field and impacts the surface of the magnetron target material, sputtering out target atoms.

[0141] (4) The plasma beam jetted from the ion source obtained in step (3) onto the substrate reacts with the target atoms sputtered by the magnetron target to form a single crystal aluminum nitride (AlN) film on the substrate.

[0142] In this embodiment, the aluminum nitride (AlN) film obtained above is also subjected to X-ray diffraction (XRD) testing, and the test results are as follows: Figure 5 As shown by Figure 5 It can be seen that the aluminum nitride (AlN) film is a single crystal film with a (002) preferred orientation.

[0143] Example 2

[0144] The magnetron sputtering coating device provided in this embodiment is different from that in Embodiment 1 only in that: in the magnetron sputtering coating device provided in this embodiment, the direction of the sample placement plane of the sample stage 4 is taken as the horizontal direction, and the placement directions of the first ion source and the second ion source are both 60° to the horizontal direction of the sample stage 4. The rest of the contents are the same as those in Embodiment 1.

[0145] The present invention also provides a magnetron sputtering coating method based on the above magnetron sputtering coating device, and the specific steps are as follows:

[0146] (1) A (100) oriented single crystal silicon wafer was used as a substrate. The single crystal silicon wafer was immersed in a 10 wt% hydrofluoric acid solution for 60 s, then ultrasonically cleaned in acetone for 20 min, then rinsed with ultrapure water, and finally dried with nitrogen to obtain a cleaned substrate.

[0147] (2) Place the cleaned silicon substrate on the hollow frame of the sample stage, and use the front-stage mechanical pump and molecular pump to evacuate the reaction chamber until the background vacuum of the reaction chamber measured by the vacuum gauge is 5×10 - 5 Pa, turn on the gas mass flow meter, set the working flow rate of the working gas argon to 10 sccm, then adjust the opening of the limiting valve, and use the gas mass flow meter and the limiting valve to adjust the working vacuum degree in the reaction chamber to 1.5 Pa.

[0148] (3) Turn on the ion source power supply, set the current of the first ion source and the second ion source to 200 mA, use the water-cooling inlet to continuously introduce cooling water into the hollow annular water-cooling groove, and then flow out from the water-cooling outlet. Use nitrogen as the reaction gas, set the nitrogen flow rate to 30 sccm, and let the nitrogen enter the two ion sources from the first air inlet in the symmetrically arranged first ion source and the second ion source respectively, and circulate through the transmission channel. In the first ion source and the second ion source, a closed magnetic field is formed by the first monopole magnet hollow column and the second monopole magnet hollow column. Under the action of the magnetic field and the inner anode ring, the nitrogen is ionized into plasma to form a plasma beam, and then reaches the outlets of the first ion source and the second ion source through the transmission channel, and is ejected onto the substrate of the sample stage under the action of the electric field.

[0149] While turning on the ion source power supply, turn on the magnetron target power supply of the high-power pulsed DC power supply, and use aluminum metal with a size of 3 inches and a purity of 99.99% as the magnetron target material. It is located in the three magnetron targets set on the bottom of the reaction chamber. The magnetron target current is set to 400W, and argon continues to enter the reaction chamber through the second gas inlet set in the reaction chamber. The flow rate of argon is maintained at 10sccm. The argon is ionized into plasma through the electric field between the magnetron target and the reaction chamber. The ionized plasma is accelerated under the action of the electric field and impacts the surface of the magnetron target material, sputtering out target atoms.

[0150] (4) The nitrogen plasma beam jetted onto the substrate from the ion source obtained in step (3) reacts with the target atoms sputtered from the magnetron target on the substrate of the substrate material obtained in step (1) to obtain a single crystal aluminum nitride (AlN) thin film.

[0151] Example 3

[0152] The difference between this embodiment and embodiment 1 is that in the magnetron sputtering coating device provided in this embodiment, the direction of the sample placement plane of the sample stage 4 is taken as the horizontal direction, and the placement directions of the first ion source and the second ion source are both 20° to the horizontal direction of the sample stage 4. The rest of the contents are the same as those in embodiment 1.

[0153] Example 4

[0154] The difference between this embodiment and embodiment 1 is that in the magnetron sputtering coating device provided in this embodiment, the direction of the sample placement plane of the sample stage 4 is taken as the horizontal direction, and the placement directions of the first ion source and the second ion source are both 80° to the horizontal direction of the sample stage 4. The rest of the contents are the same as those in embodiment 1.

[0155] Example 5

[0156] The difference between this embodiment and embodiment 1 is that in the magnetron sputtering coating device provided in this embodiment, the magnetron target power supply 12 adopts a conventional DC power supply, and the power of the magnetron target power supply during the magnetron sputtering coating process is set to 100 W. The rest of the contents are the same as those in embodiment 1.

[0157] Example 6

[0158] The difference between this embodiment and embodiment 1 is that in the magnetron sputtering coating device provided in this embodiment, the magnetron target power supply 12 adopts a conventional radio frequency power supply, and the power of the magnetron target power supply is set to 300 W during the magnetron sputtering coating process. The rest of the contents are the same as those in embodiment 1.

[0159] Example 7

[0160] The difference between this embodiment and embodiment 1 is that in the magnetron sputtering coating device provided in this embodiment, the water cooling tank 3-10, the water cooling inlet 3-11 and the water cooling outlet 3-12 are omitted. Accordingly, step (3) in the magnetron sputtering coating method provided in this embodiment omits the use of the water cooling inlet to continuously introduce cooling water into the hollow annular water cooling tank and then flow out from the water cooling outlet. The rest of the contents are the same as those in embodiment 1.

[0161] Example 8

[0162] The difference between this embodiment and embodiment 1 is that in the magnetron sputtering coating method provided in this embodiment, the nitrogen flow rate set in step (3) is 20 sccm, and the flow rate of the working gas argon is 10 sccm, that is, the ratio of the flow rate of the working gas argon to the flow rate of the reactive gas nitrogen is 1:2. The rest of the contents are the same as those in embodiment 1.

[0163] Example 9

[0164] The difference between this embodiment and embodiment 1 is that in the magnetron sputtering coating method provided in this embodiment, the nitrogen flow rate set in step (3) is 10 sccm, and the flow rate of the working gas argon is 10 sccm, that is, the ratio of the flow rate of the working gas nitrogen to the flow rate of the reaction gas nitrogen is 1:1. The rest of the contents are the same as those in embodiment 1.

[0165] Example 10

[0166] The difference between this embodiment and embodiment 1 is that in the magnetron sputtering coating method provided in this embodiment, the process adopted in step (3) includes: not turning on the ion source power supply, only passing the nitrogen reaction gas into the first ion source and the second ion source, and not using the ion source to ionize the reaction gas. The rest of the contents are the same as those in embodiment 1.

[0167] In this embodiment, the film obtained above is also subjected to X-ray diffraction (XRD) testing, and the test results are as follows: Figure 6 As shown by Figure 6 It can be seen that the prepared film is an amorphous film and does not show any preferential orientation.

[0168] Comparative Example 1

[0169] The difference between this comparative example and Example 1 is that in the magnetron sputtering coating device provided in this comparative example, the second ion source is omitted, that is, only the first ion source is provided. Accordingly, in the magnetron sputtering coating method provided in this comparative example, in step (3), only nitrogen is introduced into the first ion source from the gas inlet of the first ion source through the transmission channel, and only the first ion source is used to ionize the reaction gas nitrogen. The rest of the contents are the same as in Example 1.

[0170] Comparative Example 2

[0171] The difference between this comparative example and Example 1 is that in the magnetron sputtering coating device provided in this comparative example, the symmetrically arranged first ion source and the second ion source are omitted. Accordingly, the steps (3) and (4) of the magnetron sputtering coating method provided in this comparative example only include the following steps:

[0172] The magnetron target power supply of the high-power pulsed DC power supply is turned on. A 3-inch aluminum nitride target with a purity of 99.99% is used as the magnetron target material. The target is located in the three magnetron targets arranged on the bottom surface of the reaction chamber. The magnetron target power is set to 200 W. Argon gas continues to enter the reaction chamber through the second gas inlet arranged in the reaction chamber. The flow rate of argon gas is maintained at 10 sccm. The argon gas is ionized into plasma by the electric field between the magnetron target and the reaction chamber. The ionized plasma is accelerated under the action of the electric field and collides with the surface of the magnetron target material, sputtering target material atoms to form a thin film on the substrate material obtained in step (1). The rest of the contents are the same as those in Example 1.

[0173] In this comparative example, the film obtained above was also subjected to X-ray diffraction (XRD) testing, and the test results are as follows: Figure 7 As shown by Figure 7 It can be seen that the prepared film is an amorphous film and does not show any preferential orientation.

[0174] The magnetron sputtering coating devices and the prepared films provided in the above Examples 1-10 and Comparative Examples 1-2 were subjected to the following tests:

[0175] (1) Thin film deposition rate: The thickness of the thin film deposited on the substrate for a certain period of time is directly tested using a step profiler (model KOSAKA ET200A). Then, the deposition rate of the thin film is calculated, where the deposition rate of the thin film = film thickness / film deposition time.

[0176] (2) Volume concentration of the ionized plasma of the reaction gas: The volume concentration of the reaction gas plasma in the reaction chamber is directly measured using a Langmuir probe.

[0177] (3) Al:N stoichiometric ratio: Test the stoichiometric ratio of aluminum and nitrogen in the final film. The test results are shown in Table 1:

[0178] Table 1

[0179]

[0180] The test results show that:

[0181] (1) It can be seen from Examples 1 to 2 that the present invention arranges symmetrical dual ion sources on the two end sides of the reaction chamber, and arranges a magnetron target on the bottom surface of the reaction chamber, and adopts the symmetrically arranged dual ion sources to directly ionize the reaction gas in conjunction with the sputtering of the magnetron target arranged at the bottom of the device, and performs reaction coating on the substrate at the sample stage at the top of the device, thereby increasing the ionization content of the reaction gas, suppressing the target poisoning phenomenon during sputtering, and the ionized gas directly reacts with the sputtered target material, thereby increasing the coating deposition rate of the substrate material, and realizing the preparation of crystalline thin films at low temperatures.

[0182] (2) By comparing Example 1 with Examples 3-4, it can be seen that the present invention can further increase the reaction efficiency between the ionized reaction gas and the target atoms sputtered by the magnetron target by further adjusting the placement direction of the ion source so that it has a fixed angle with the direction of the sample placement plane of the sample stage, thereby avoiding the etching of the thin film on the surface of the substrate by the ion beam emitted by the ion source, thereby ensuring the quality of the thin film. In the present invention, if the angle between the placement direction of the ion source and the horizontal direction of the sample stage is too small, the ionization efficiency of the ion source for the reaction gas will not be affected, but the deposition rate will eventually decrease due to the small amount of plasma shot toward the sample stage; if the angle is too large, most of the plasma beam of the reaction gas ionized by the ion source will be shot toward the surface of the substrate, causing etching of the substrate thin film, reducing the deposition rate of the thin film and causing the surface of the thin film to be porous, thereby reducing the quality of the thin film and causing the atomic weight ratio of the thin film to be too large.

[0183] (3) By comparing Example 1 with Examples 5-6, it can be seen that, compared with conventional DC power supplies and conventional RF power supplies, the use of a high-power pulse power supply as a magnetron target power supply can improve the reaction rate of the magnetron sputtering coating device, and cooperate with the symmetrically arranged dual ion source to accelerate the coating speed of the device.

[0184] (4) It can be seen from the comparison between Example 1 and Example 7 that if the water cooling tank is omitted in the magnetron sputtering coating device provided by the present invention, the ion source will overheat during operation, the magnet will demagnetize, and eventually the ion source will automatically extinguish and fail to work.

[0185] (5) By comparing Example 1 with Examples 8-9, it can be seen that the present invention controls the ratio of the flow rate of the working gas to the flow rate of the reaction gas, which can adjust the atomic stoichiometric ratio of the prepared film and also affect the deposition rate.

[0186] (6) By comparing Example 1 with Example 10, it can be seen that if the present invention omits the symmetrically arranged first ion source and the second ion source, and instead adopts a method of directly introducing the reaction gas into the reaction chamber through the ion source air inlet, the reaction gas has a low ionization content and a low ionization rate. When the reaction gas reacts with the aluminum atoms sputtered by the magnetron target to prepare a thin film, the stoichiometric ratio of the prepared thin film will be greatly different, the deposition rate will be reduced, and the prepared thin film will not have any preferentially oriented amorphous state.

[0187] (7) It can be seen from the comparison between Example 1 and Comparative Example 1 that if the magnetron sputtering coating device of the present invention lacks the second ion source, the deposition rate will decrease.

[0188] (8) By comparing Example 1 with Comparative Example 2, it can be seen that if the symmetrically arranged first ion source and second ion source are omitted in the present invention, and an aluminum nitride target is used as a magnetron target material to be directly sputtered onto a substrate material to prepare a thin film, the prepared thin film will also not have any preferentially oriented amorphous state, and the deposition rate will be slower.

[0189] In summary, the magnetron sputtering coating device provided by the present invention sets the sample stage at the top of the reaction chamber, sets the magnetron target at the bottom of the reaction chamber, and sets symmetrical dual ion sources on the two end sides of the reaction chamber. The dual ion sources symmetrically set at the two ends of the device are used to ionize the reaction gas and cooperate with the target material sputtering of the magnetron target at the bottom of the device to perform reactive sputtering film formation on the substrate on the top sample stage. The target material atoms sputtered by the magnetron target directly react with the plasma state of the ionized reaction gas ejected by the ion source flow, thereby improving the reaction efficiency and rate between the plasma beam of the ionized reaction gas and the sputtered target material atoms. In addition, directly introducing the reaction gas into the ion source for ionization can significantly improve the ionization content of the reaction gas, and can effectively suppress target poisoning during the reactive sputtering process, thereby improving the reactive sputtering rate of the coating device.

[0190] The applicant declares that the above is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention shall fall within the protection scope and disclosure scope of the present invention.

Claims

1. A magnetron sputtering coating device, It is characterized in that The magnetron sputtering coating device comprises a reaction chamber, a magnetron target, an ion source and a sample stage; The reaction chamber is a vacuum sealing structure; The magnetron target is fixed and connected to the bottom surface of the reaction chamber; The ion source comprises a first ion source and a second ion source which are symmetrically arranged, wherein the first ion source and the second ion source are respectively fixed and connected to the two end sides of the reaction chamber; the ion source comprises a first gas inlet, a transmission channel and an outlet, wherein the first gas inlet is used to introduce a reaction gas from the outside of the reaction chamber into the ion source; The sample stage is located at the top of the reaction chamber.

2. The magnetron sputtering coating device according to claim 1, It is characterized in that The sides of both ends of the reaction chamber are provided with fixing components for fixing the ion source; Taking the direction of the sample placement plane of the sample stage as the horizontal direction, the placement directions of the first ion source and the second ion source are both 30-60° to the horizontal direction of the sample stage; The ion source includes an anode layer ion source.

3. The magnetron sputtering coating device according to claim 2, It is characterized in that The ion source also includes an electromagnetic shield; A connecting shaft is provided in the central area of ​​the bottom surface of the electromagnetic shielding cover, and the connecting shaft is fixed and connected to the bottom surface of the electromagnetic shielding cover and extends to the outside of the bottom surface; In the magnetron sputtering coating device, a connecting shaft extending to the outside of the electromagnetic shielding cover of the ion source is connected to the fixing components arranged on the two end sides of the reaction chamber, so that the ion source is fixed and connected to the two end sides of the reaction chamber; A first monopole magnet hollow column is also arranged on the inner bottom surface of the electromagnetic shielding cover, and a second monopole magnet hollow column is arranged on the upper end of the first monopole magnet hollow column, and the first monopole magnet hollow column and the second monopole magnet hollow column both surround and are fixed to the side of the connecting shaft; An inner anode ring is arranged on the outer side of the second monopole magnet hollow column away from the connecting shaft.

4. The magnetron sputtering coating device according to claim 3, It is characterized in that A water cooling groove is also provided inside the electromagnetic shielding cover, and the water cooling groove is located outside the hollow column of the first monopole magnet away from the connecting shaft; The bottom of the water cooling tank is also provided with a water cooling inlet and a water cooling outlet; The lower ends of the water cooling inlet and the water cooling outlet extend outward to the outside of the bottom surface of the electromagnetic shielding cover and are connected to the bottom surface of the electromagnetic shielding cover; The first air inlet in the ion source is connected to the bottom surface of the electromagnetic shield and extends to the outside of the bottom surface; The ion source further comprises a power supply interface, the upper end of which is connected to the inner anode ring, and the lower end of which is connected to the bottom surface of the electromagnetic shielding cover and extends to the outside of the bottom surface.

5. The magnetron sputtering coating device according to claim 1, It is characterized in that The magnetron sputtering coating device also includes an ion source power supply and a magnetron target power supply located outside the reaction chamber; The ion source power supply is connected to a power supply interface in the ion source; The magnetron target power supply is connected to the magnetron target; The magnetron target power supply includes any one of a high-power pulse power supply, a radio frequency power supply or a direct current power supply, or a combination of at least two of them.

6. The magnetron sputtering coating device according to claim 1, It is characterized in that The reaction chamber is provided with a second gas inlet for introducing the working gas into the reaction chamber; The magnetron sputtering coating device also includes a servo motor located outside the top surface of the reaction chamber; The servo motor passes through the top surface of the reaction chamber through a connecting channel and is connected to a connecting rod on the sample stage, so as to drive the rotation of the sample stage; The connecting channel in the servo motor and the connecting rod on the sample stage are driven by a transmission element.

7. The magnetron sputtering coating device according to claim 1, It is characterized in that The magnetron sputtering coating device further includes a vacuum gauge disposed outside the reaction chamber, for measuring the vacuum degree in the reaction chamber; The magnetron sputtering coating device also includes an observation window arranged on the side of the reaction chamber for observing the sputtering process; The magnetron sputtering coating device also includes a pump group, a flow limiting valve and a gas mass flow meter, which are used to obtain and control the vacuum degree of the reaction chamber; The pump group includes a front-stage mechanical pump and / or a molecular pump.

8. A magnetron sputtering coating method based on the magnetron sputtering coating device according to any one of claims 1 to 7, It is characterized in that The specific process of the magnetron sputtering coating method includes: A substrate is placed on a sample stage, and a reaction chamber is evacuated; reaction gases are introduced into the two ion sources from the first air inlets of the symmetrically arranged first ion source and the second ion source, respectively, and circulated through the transmission channel. In the two ion sources, the reaction gases are ionized into plasma to form a plasma beam, and then reach the outlets of the two ion sources through the transmission channel, and are ejected onto the substrate under the action of an electric field; at the same time, a magnetron target material in the magnetron target is sputtered into target material atoms; the target material atoms react with the plasma beam ejected onto the substrate, and a thin film is deposited and prepared on the substrate.

9. The magnetron sputtering coating method according to claim 8, It is characterized in that The thin film prepared on the base substrate is any one of a single crystal thin film and a polycrystalline thin film; During the vacuuming process, the reaction chamber is evacuated by a pump group until the background vacuum degree of the reaction chamber is 8×10 -5 Below Pa; After the vacuuming, the magnetron sputtering coating method further comprises introducing a working gas into the reaction chamber, and adjusting the working vacuum degree in the reaction chamber to 0.5-1.5 Pa by using a gas mass flow meter and a flow limiting valve; During the ionization process, the current of the first ion source and the second ion source is set to 50-300 mA.

10. The magnetron sputtering coating method according to claim 8, It is characterized in that The specific process of sputtering the magnetron target material into target material atoms includes: introducing a working gas into the reaction chamber through a second gas inlet provided in the reaction chamber, and ionizing the working gas into plasma through an electric field between the magnetron target and the reaction chamber, wherein the plasma is accelerated under the action of the electric field and collides with the surface of the magnetron target material in the magnetron target, thereby sputtering out the target material atoms; The working gas includes an inert gas; The ratio of the flow rate of the working gas to the flow rate of the reaction gas is 1:(1-3).

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