CN115386848A - Multi-target direct-current magnetron sputtering film coating device and application thereof in depositing ceramic substrate multilayer metal film - Google Patents
Multi-target direct-current magnetron sputtering film coating device and application thereof in depositing ceramic substrate multilayer metal film Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
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Abstract
The invention discloses a multi-target direct current magnetron sputtering film coating device and application thereof in depositing a ceramic substrate multi-layer metal film. The structure of the multi-target direct current magnetron sputtering device is as follows: a workpiece frame is arranged at the bottom in the coating chamber, and first to fifth targets, an ion source and a heating pipe are arranged at the upper part of the workpiece frame; the top of the coating chamber is provided with a three-flow meter; the vacuum pumping system comprises a rough pumping system and a fine pumping system and is used for vacuumizing the coating chamber; the measuring system comprises a first thermocouple sensor and a second thermocouple vacuum gauge which are arranged on the film coating chamber; the control system includes a first thermocouple vacuum gauge control unit, a first molecular pump controller, first through fifth sputtering target power supplies, a first ion source power supply, and a first bias power supply. The multi-target direct current magnetron sputtering device is utilized to deposit a plurality of metal films on the surface of the large-size special-shaped zirconia ceramic, so that the surface modification of the zirconia ceramic is realized, the surface outgassing rate and the resolution rate of the zirconia ceramic can be reduced, and the zirconia ceramic has higher conductivity.
Description
Technical Field
The invention relates to a multi-target direct current magnetron sputtering film coating device and application thereof in depositing a ceramic substrate multi-layer metal film, belonging to the technical field of surfaces.
Background
Aiming at the forefront of international heavy ion scientific research, a high-current Heavy Ion Accelerator (HIAF) developed by modern physical research institute of Chinese academy of sciences is a large scientific engineering device with full-particle acceleration capability and can provide a pulse heavy ion beam current of up to 4.25 GeV/u. In order to meet the requirement of beam current service life, the vacuum degree of a BRIng vacuum system is required to be superior to 1 multiplied by 10 -9 Pa. At the same time, in order to reduce the rapidly changing magnetic field in the corresponding vacuumThe eddy current effect generated on the chamber further reduces the thickness of the vacuum chamber. When the wall thickness of the vacuum chamber is small (0.3 mm) and the vacuum degree is extremely high (10) -9 Pa), the difference between the vacuum chamber and the atmospheric pressure is 15 orders of magnitude, and the thin-wall vacuum chamber can deform under the action of the atmospheric pressure. In order to counteract the deformation, a ceramic-lined thin-walled vacuum chamber structure with a thickness of 0.3mm is proposed, which uses zirconia ceramic material as an internal support of the vacuum chamber to prevent the deformation of the vacuum chamber under atmospheric pressure. Zirconia ceramics have the advantages of high strength, hardness, and good toughness and wear resistance, and are therefore often used as structural materials, and are considered to be the most promising new structural materials. Meanwhile, the crystal structure of the zirconia material is stable within 300 ℃, volume expansion cannot be generated by tetragonal monoclinic transformation, volume contraction cannot be generated by monoclinic tetragonal transformation, and the requirement of ultrahigh vacuum obtaining on baking conditions is met. However, zirconia ceramics have a disadvantage of high outgassing rate and desorption rate. In order to solve the problem, a multi-target direct current magnetron sputtering device is designed, and a multilayer film is deposited on the surface of large-size special-shaped zirconia ceramic to modify the surface of the ceramic so as to meet the requirements (low outgassing rate, low desorption rate and high conductivity) of a magnet on a vacuum chamber in the physical design of an accelerator.
Disclosure of Invention
The invention aims to provide a multi-target direct current magnetron sputtering device, which realizes surface modification of zirconia ceramics by depositing a plurality of metal films on the surface of large-size special-shaped zirconia ceramics, can reduce the surface outgassing rate and the resolution rate of the zirconia ceramics and simultaneously has higher conductivity.
The invention provides a multi-target direct current magnetron sputtering device which comprises a coating chamber, a vacuum pumping system, a measuring system and a control system;
a first workpiece frame is arranged at the bottom in the coating chamber, and a first sputtering target, a second sputtering target, a first ion source, a first heating pipe, a third sputtering target, a fourth sputtering target and a fifth sputtering target are arranged at the upper part of the first workpiece frame; the top of the coating chamber is provided with a first flowmeter, a second flowmeter and a third flowmeter;
the vacuum pumping system comprises a rough pumping system and a fine pumping system and is used for vacuumizing the coating chamber;
the measuring system comprises a first thermocouple sensor and a second thermocouple vacuum gauge which are arranged on the film plating chamber, and a first thermocouple vacuum gauge which is arranged on the rough pumping system and is used for measuring the vacuum degree and temperature change of the film plating chamber; specifically, the first thermocouple vacuum gauge is used for measuring the vacuum degree of a preceding stage system, the second thermocouple vacuum gauge is used for measuring the vacuum degree in the coating chamber, and the measurement range is (1 atm-1 × 10) -5 Pa), the first thermocouple sensor is used for measuring the temperature change in the coating chamber;
the control system comprises a first thermocouple vacuum gauge control unit, a first molecular pump controller, a first sputtering target power supply, a second sputtering target power supply, a third sputtering target power supply, a fourth sputtering target power supply, a first ion source power supply and a first bias power supply, wherein the first molecular pump controller is used for controlling a first molecular pump arranged on the fine pumping system.
In the multi-target dc magnetron sputtering apparatus, the rough pumping system includes a first vane pump, a first roots pump, the first thermocouple vacuum gauge, a fifth valve, and a sixth valve.
In the multi-target dc magnetron sputtering apparatus, the fine pumping system includes a second rotary vane pump, a first valve, the first molecular pump, a second valve, and a third valve;
the rough pumping system is communicated with the fine pumping system, and a fourth valve is arranged on a communicated pipeline.
In the multi-target direct current magnetron sputtering device, the first valve, the second valve, the third valve and the fifth valve are all pneumatic vacuum valves;
the third valve is a pneumatic high valve and is used for adjusting the air extraction angle, and the physical mechanism is that the pumping speed of the fine pumping unit is controlled by adjusting the size of the flow guide;
the sixth valve is a pneumatic air release valve and aims to release the vacuum state of the coating chamber.
In the multi-target direct current magnetron sputtering device, the first sputtering target, the second sputtering target, the fourth sputtering target and the fifth sputtering target are cylindrical targets with a height of 800-1000 mm, and the higher the height of the sputtering target, the wider the coverage area is, which is beneficial to batch coating;
the third sputtering target is a plane target with the height of 600-800 mm;
each sputtering target is provided with a pneumatic baffle plate, which aims to ensure that the non-working target is polluted and can clean the target when the target baffle plate is closed.
In the multi-target dc magnetron sputtering apparatus, the first sputtering target power supply, the second sputtering target power supply, and the fourth sputtering target power supply are 20KW dc power supplies; the power supply of the third sputtering target is a 30KW direct current power supply, and the fifth sputtering target and the third sputtering target share the power supply; the first ion source power supply provides stable voltage output for the first ion source to work, and when Ar gas is filled in the film coating chamber and the stable working air pressure is maintained, the first ion source can generate stable Ar plasma which can be used for cleaning the surface of a substrate, so that the surface is activated, and film deposition is facilitated. Meanwhile, ar ions provide stable sputtering energy for the sputtering target material; the first bias power supply provides stable negative bias for the substrate, so that the bonding force of a deposited film layer can be improved, the roughness can be reduced and the like; the measuring ranges of the first flowmeter, the second flowmeter and the third flowmeter are all 1000SCCM, and the first flowmeter, the second flowmeter and the third flowmeter are mainly used for controlling working gas Ar and reaction gas N 2 Etc. flow size; the first workpiece frame can realize revolution and autorotation of workpieces, is beneficial to depositing uniform film layers, and can perform simultaneous film coating on 48 ceramic rings.
The multi-target direct current magnetron sputtering device also comprises a cooling system which can provide 4 kg of water pressure and is used for cooling the target material, the pump set and the like.
On the basis of the multi-target direct current magnetron sputtering device, the invention also provides a method for depositing a Ti-Cu-Ti-Au multilayer film on a substrate, which comprises the following steps:
s1, preprocessing a substrate, and specifically comprises the following steps: ultrasonic cleaning with isopropanol for 20min, ultrasonic cleaning with deionized water for 20min, and vacuum oven drying at 100 deg.C;
s2, mounting the substrate on the first workpiece frame in the multi-target direct current magnetron sputtering device, and closing a furnace door; starting the rough pumping system and the fine pumping system to perform rough pumping and fine pumping on the coating chamber in sequence, and closing the rough pumping system when the pressure in the coating chamber reaches a preset value;
s3, introducing high-purity argon into the coating chamber through the first flowmeter; starting the first heating pipe to heat the zirconia ceramics, and starting the first ion source to perform plasma bombardment cleaning on the surface of the substrate;
s4, closing the ion source, starting the first sputtering target power supply and the second sputtering target power supply, and depositing a first layer of Ti on the surface of the substrate by using the first sputtering target and the second sputtering target;
s5, turning off the first sputtering target power supply and the second sputtering target power supply, turning on the fourth sputtering target power supply and the fifth sputtering target power supply, and depositing a second layer of Cu on the surface of the substrate by using the fourth sputtering target and the fifth sputtering target;
s6, turning off the fourth sputtering target power supply and the fifth sputtering target power supply, turning on the first sputtering target power supply and the second sputtering target power supply, and depositing a third layer of Ti on the surface of the substrate by using the first sputtering target and the second sputtering target;
s7, turning off the first sputtering target power supply and the second sputtering target power supply, turning on the third sputtering target power supply, and depositing a fourth layer of Au on the surface of the substrate by using the third sputtering target;
and S8, closing the third sputtering target power supply, the first heating pipe, the first bias power supply, the rough pumping system and the fine pumping system, and filling argon for cooling to obtain the Ti-Cu-Ti-Au multilayer film on the substrate.
In the above method, in step S2, the film plating chamber is rough pumped and fine pumped as follows:
opening the first rotary vane pump and the fifth valve, roughly pumping the film coating chamber until the indication number of the first thermocouple vacuum gauge is less than 5 multiplied by 10 2 When Pa, the first roots pump is started; simultaneously opening the second vane pump, the second valve and the first molecular pump; after the molecular pump is started normally and the reading of the second thermocouple vacuum gauge is less than 1Pa, opening the second valve and finely pumping the film coating chamber;
the pressure in the film coating chamber is lower than 8 x 10 -3 And after Pa, closing the fifth valve, the first roots pump and the first rotary vane pump.
In the method, in the step S3, the heating temperature is 150-200 ℃ and the time is 60-120 min;
when plasma bombardment cleaning is carried out, the bias voltage is controlled to be 0-200V and 0-99 percent;
in step S4, before deposition, the air exhaust angle of the third valve is adjusted to 0-90 degrees, the pressure of the film coating chamber is controlled to 0.1-1 Pa, the bias voltage is controlled to 0-200V, and the bias voltage is 0-99%.
In the above method, in step S4, the currents of the first sputtering target power supply and the second sputtering target power supply are 10 to 15A;
the deposition time is 5-20 min, the bias voltage is 0-200V, 0-99%;
in step S5, the currents of the fourth sputtering target power supply and the fifth sputtering target power supply are 10 to 15A;
the deposition time is 30-60 min, the bias voltage is 0-200V, 0-99%;
in step S6, the currents of the first sputtering target power supply and the second sputtering target power supply are 10 to 15A;
the deposition time is 5-20 min, the bias voltage is 0-200V, 0-99%;
in step S7, the current of the third sputtering target power supply is 3-5A;
the deposition time is 30-120 min.
In the above method, after step S8, the method further includes the following step of additionally plating Au:
repeating the step S2, and opening the first heating pipe to preheat the workpiece; introducing high-purity argon, and adjusting the air extraction angle by adjusting the third valve; and repeating the step S7 to perform Au coating.
The first sputtering target and the second sputtering target adopted by the method are Ti targets with the purity of 99.99 percent; the fourth sputtering target and the fifth sputtering target are cu targets having a purity of 99.99%; the third sputtering target was an Au target having a purity of 99.99%.
The Ti-Cu-Ti-Au multilayer film with the substrate prepared by the method has good film thickness uniformity, bonding force and the like.
The substrate can be a ceramic substrate, a stainless steel substrate or a titanium alloy substrate;
the ceramic substrate may be a zirconia ceramic substrate, an alumina ceramic substrate, or a silicon nitride ceramic substrate.
Specifically, in the zirconia ceramic substrate, the first layer of Ti is plated to increase the film-base bonding force between the film and the zirconia surface, the thermal expansion coefficient of Ti and the zirconia is similar, and Ti and Zr can be replaced at the interface; the second layer of plated Cu is for cost saving (Au has characteristics of small surface desorption rate and high conductivity), and as is known, cu has good conductivity and low cost, and the plated Cu is for reducing the thickness of the fourth layer of Au film; the Cu ions have very high activity and are easy to migrate to the surrounding environment, so the purpose of the third layer Ti plating is to separate the Cu film from the Au film, avoid the migration of the Cu crystal phase to the Au crystal phase and ensure that the Au film on the surface layer is impure. The last layer of Au film is used for reducing the gas release rate and the desorption rate of the surface of the zirconia ceramic and ensuring that the change of the pressure in the vacuum chamber in the idle load and the running of the accelerator is within an acceptable range.
The invention has the following beneficial technical effects:
(1) In terms of the apparatus; the multi-target direct current magnetron sputtering device can realize that multiple sputtering targets deposit multiple layers of films in the first coating chamber at one time, and has the functions of ion source cleaning and bias control;
(2) In the context of multilayer film deposition processes; a method for depositing a Ti-Cu-Ti-Au multilayer film on a large-size special-shaped zirconia ceramic substrate is a surface treatment method for reducing the eddy effect of a vacuum chamber in an accelerator vacuum system and maintaining dynamic vacuum at a stable level for the first time.
Drawings
FIG. 1 is a schematic structural diagram of a multi-target DC magnetron sputtering apparatus according to the present invention.
The labels in the figure are as follows:
1-a first rotary vane pump, 2-a first roots pump, 3-a second rotary vane pump, 4-a first valve, 5-a first molecular pump, 6-a second valve, 7-a third valve, 8-a fourth valve, 9-a first thermocouple vacuum gauge, 10-a fifth valve, 11-a sixth valve, 12-a first sputtering target, 13-a second sputtering target, 14-a first ion source, 15-a first heating pipe, 16-a third sputtering target, 17-a fourth sputtering target, 18-a fifth sputtering target, 19-a first workpiece holder, 20-a first coating chamber, 21-a first thermocouple sensor, 22-a first flowmeter, 23-a second flowmeter, 24-a third flowmeter, 25-a second thermocouple vacuum gauge, 26-a first thermocouple vacuum control unit, 27-a first molecular pump controller, 28-a first sputtering target, 29-a second sputtering target power supply, 30-a third thermocouple power supply, 31-a fourth power supply, 32-a first target vacuum control unit, and 33-a first bias ion source.
FIG. 2 is a photograph of a Ti-Cu-Ti-Au multilayer film deposited on a zirconia ceramic ring substrate according to an embodiment of the present invention.
FIG. 3 shows AFM and surface roughness test results of Ti-Cu-Ti-Au multilayer films deposited on a zirconia ceramic ring substrate according to an embodiment of the present invention, wherein the left graph is an AFM surface topography graph, and the right graph is a surface roughness result.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1 Multi-target DC magnetron sputtering apparatus
As shown in FIG. 1, the multi-target DC magnetron sputtering apparatus provided by the invention comprises a coating chamber, a vacuum pumping system, a measurement system, a cooling system and a control system. The main body of the coating chamber is a first coating chamber 20, and is provided with a first sputtering target material 12, a second sputtering target material 13, a first ion source 14, a first heating pipe 15, a third sputtering target material 16, a fourth sputtering target material 17, a fifth sputtering target material 18, a first workpiece holder 19, a first flowmeter 22, a second flowmeter 23, a third flowmeter 24 and the like. The vacuum pumping system comprises a rough pumping system and a fine pumping system, wherein the rough pumping system comprises a first rotary vane pump 1 and a first Roots pump 2, the fine pumping system comprises a second rotary vane pump 3, a first valve 4 and a first molecular pump 5, and the vacuum system can enable the pressure in the first coating chamber 20 to reach 8 x 10 within 15min -3 Pa after Pa, ultimate vacuum of 3X 10 -4 Pa. The measuring system comprises a first thermocouple vacuum gauge 9, a second thermocouple vacuum gauge 25 and a first thermocouple 21, and can accurately measure the vacuum degree and temperature change condition in the first coating chamber. The cooling system can provide 4 kilograms of water pressure and is used for cooling the target material, the pump set and the like. The control system comprises a first thermocouple vacuum gauge control unit 26, a first molecular pump controller 27, a first sputtering target power supply 28, a second sputtering target power supply 29, a third sputtering target power supply 30, a fourth sputtering target power supply 31, a first ion source power supply 32, a first bias power supply 33 and the like, and can adjust the target working voltage, the first heating pipe heating power and the like in real time through a control panel.
As shown in fig. 1, the first valve 4, the second valve 6, the fourth valve 8 and the fifth valve 10 are all pneumatic vacuum valves; the third valve is a pneumatic high valve 7 and is used for adjusting the air extraction angle, and the physical mechanism is that the pumping speed of the fine pumping unit is controlled by adjusting the flow conductance; the sixth valve 11 is a pneumatic relief valve for relieving the vacuum state of the first coating chamber.
As shown in fig. 1, a first thermocouple vacuum gauge 9 is used to measure the backing system vacuum; the second thermocouple vacuum gauge 25 is used for measuring the vacuum degree in the first coating chamber, and the measurement range is (1 atm-1 multiplied by 10) -5 Pa); first of allThe thermocouple sensor 21 is used to measure the temperature change in the first coating chamber.
As shown in fig. 1, the first sputtering target 12, the second sputtering target 13, the fourth sputtering target 17, and the fifth sputtering target 18 are cylindrical targets having a height of 800mm; the third sputtering target 14 is a planar target, and the height is also 800mm; the higher the height of the sputtering target material is, the wider the coverage area is, which is beneficial to batch coating; each sputtering target is provided with a pneumatic baffle plate, which aims to ensure that the non-working target is polluted and can clean the target when the target baffle plate is closed. The corresponding first sputtering target power supply 28, second sputtering target power supply 29 and fourth sputtering target power supply 31 are 20KW direct current power supplies; the third sputtering target power supply 30 is a 30KW direct current power supply, and the fifth sputtering target 18 and the third sputtering target 14 share the power supply; the first ion source power supply 32 provides a stable voltage output for the ion source operation, and when the first coating chamber 20 is filled with Ar gas and maintained at a stable operating pressure, the ion source can generate a stable Ar plasma, which can be used to clean the substrate surface, thereby activating the surface and facilitating the film deposition. Meanwhile, ar ions provide stable sputtering energy for the sputtering target material; the first bias power supply 33 provides a stable negative bias for the substrate, which can improve the bonding force of the deposited film, reduce the roughness and the like; the measuring ranges of the first flowmeter 22, the second flowmeter 23 and the third flowmeter 24 are all 1000sccm, and the first flowmeter, the second flowmeter and the third flowmeter are mainly used for controlling the flow of the working gas Ar, the reaction gas N2 and the like; the first workpiece holder 19 can realize revolution and rotation of the workpiece, which is beneficial to depositing a uniform film layer, and can perform simultaneous film coating of 48 ceramic rings.
Further testing the designed multi-target DC magnetron sputtering device, the ultimate vacuum degree of the device system is 3 multiplied by 10 -4 Pa; the first ion source 14, the first sputtering target 12, the second sputtering target 13, the third sputtering target 16, the fourth sputtering target 17, the fifth sputtering target 18 and the like all work stably; the first and second sputtering targets 12, 13 were ti targets with a purity of 99.99% during the test; the fourth and fifth sputtering targets 17 and 18 are Cu targets having a purity of 99.99%; the third sputtering target 16 was an au target with a purity of 99.99%; meanwhile, the zirconia ceramic substrate is subjected to multilayer film deposition, and films thereofThe thickness uniformity, the binding force and the like are good.
EXAMPLE 2 deposition of a zirconium oxide ceramic substrate Ti-Cu-Ti-Au multilayer film
In this embodiment, a Ti-Cu-Ti-Au multilayer film is deposited on a zirconia ceramic substrate, wherein the first layer is plated with Ti to increase the film-based bonding force between the film and the zirconia surface, the thermal expansion coefficient of Ti and zirconia is similar, and Ti and Zr can be replaced at the interface; the second layer of plated Cu is used for saving cost (Au has the characteristics of small surface desorption rate and high conductivity), and the Cu has good conductivity and lower cost, wherein the plated Cu is used for reducing the thickness of the fourth layer of Au film; the Cu ions have very high activity and are easy to migrate to the surrounding environment, so the purpose of the third layer Ti plating is to separate the Cu film from the Au film, avoid the migration of the Cu crystal phase to the Au crystal phase and ensure that the Au film on the surface layer is impure. The last layer of Au film is used for reducing the gas release rate and the desorption rate of the surface of the zirconia ceramic and ensuring that the change of the pressure in the vacuum chamber in the idle load and the running of the accelerator is within an acceptable range.
Depositing a Ti-Cu-Ti-Au multilayer film according to the following steps:
1) Firstly, zirconium oxide ceramic is pretreated by isopropanol ultrasonic cleaning for 20min, deionized water ultrasonic cleaning for 20min and drying in a vacuum furnace at 100 ℃.
2) The cleaned zirconia ceramic pieces were mounted on the first work rest 19 in the first coating chamber 20, and the oven door was closed. Opening the first rotary vane pump 1 and the fifth valve 10 to perform rough pumping on the first film coating chamber 20 until the reading of the first thermocouple vacuum gauge 9 is less than 5 multiplied by 10 2 Pa, the first roots pump 2 is turned on. Simultaneously opening the second rotary vane pump 3, the second valve 4 and the first molecular pump 5; and after the molecular pump is started normally and the reading of the second thermocouple vacuum gauge 25 is less than 1Pa, opening the second valve 6 and finely pumping the first film coating chamber 20. The pressure in the first film coating chamber is lower than 8 multiplied by 10 -3 And after Pa, closing the fifth valve 10, the first roots pump 2 and the first rotary vane pump 1.
3) The first flow meter 22 was opened, and 100sccm of high purity argon gas was introduced, and the working pressure was maintained at 0.2Pa. And opening the first heating pipe 15, and heating the workpiece at 150 ℃ for 100 min. Meanwhile, the first ion source 14 is turned on, the working voltage is adjusted to 1800V, and the surface of the workpiece is cleaned by plasma bombardment. The substrate bias was 100V,30%.
4) The first ion source 14 and the corresponding baffle are closed, the pumping angle of the third valve 7 is adjusted to 30 degrees, the pressure of the first film coating chamber 20 is 0.4Pa, and the bias voltage is controlled to 50V 30%.
5) Adjusting the currents of the first sputtering target power supply 28 and the second sputtering target power supply 29 to be 15A (the operation sequence is baffle opening, rotation opening and opening), depositing a first layer of Ti, wherein the deposition time is 10min, and the substrate bias voltage is 100V and 30%;
6) The first sputtering target power supply 28, the second sputtering target power supply 29, and the corresponding shutter plate are turned off.
7) The current of the fourth sputtering target material power supply 31 and the current of the fifth sputtering target material power supply 30 are adjusted to be 15A (the operation sequence is baffle opening, rotation opening and opening), the second layer of Cu is deposited, the deposition time is 60min, and the substrate bias voltage is 100V and 30%.
8) The fourth sputtering target power supply 31 and the fifth sputtering target power supply 30 were turned off, and the corresponding shutter plate was turned off.
9) The first sputtering target power supply 28 and the second sputtering target power supply 29 were adjusted to have a current of 15A (operation sequence of opening the shutter, opening rotation, and opening), and a third layer of Ti was deposited for 10min with a substrate bias of 100v,30%.
10 Adjusting the current of the power supply 30 of the third sputtering target to 5A, depositing the fourth layer of Au for 40min, and the operation sequence is that the baffle of the third sputtering target is opened, the power supply is turned on, and the third sputtering target moves (the target-base distance is changed).
11 Turn off the third sputtering target power supply 30, turn off the corresponding shutter, turn off the heating control, turn off the bias power supply, turn off the fine pumping valve, and charge Ar to assist in cooling.
12 Step 2) is repeated and the first heating tube 15 is opened and the workpiece is preheated at 100 c for 60 min. 120sccm of high-purity argon gas is introduced, and the pumping angle is adjusted to 30 degrees by adjusting the third valve 7.
13 Au plating is performed on the workpiece, the current of the third sputtering target material power supply 30 is adjusted to be 5A, the time is 30min, and the operation sequence is that the third sputtering target material baffle is opened, the power supply is turned on, and the workpiece is moved (the target-base distance is changed).
FIG. 2 is a photograph of a Ti-Cu-Ti-Au multilayer film deposited on a zirconia ceramic ring substrate according to this example.
The properties of the Ti-Cu-Ti-Au multilayer film prepared in this example were analyzed, and the film-zirconia base bonding force was 19.57MPa (-F =61.45n, s =3.14 × 10) -6 m 2 ) The surface roughness was better than 6nm and the film uniformity was very consistent, and the results of the AFM and surface roughness tests are shown in fig. 3.
Claims (12)
1. A multi-target direct current magnetron sputtering device comprises a coating chamber, a vacuum pumping system, a measuring system and a control system; the method is characterized in that:
a first workpiece frame is arranged at the bottom in the coating chamber, and a first sputtering target, a second sputtering target, a first ion source, a first heating pipe, a third sputtering target, a fourth sputtering target and a fifth sputtering target are arranged at the upper part of the first workpiece frame; the top of the coating chamber is provided with a first flowmeter, a second flowmeter and a third flowmeter;
the vacuum pumping system comprises a rough pumping system and a fine pumping system and is used for vacuumizing the coating chamber;
the measuring system comprises a first thermocouple sensor and a second thermocouple vacuum gauge which are arranged on the film plating chamber, and a first thermocouple vacuum gauge which is arranged on the rough pumping system and is used for measuring the vacuum degree and temperature change of the film plating chamber;
the control system comprises a first thermocouple vacuum gauge control unit, a first molecular pump controller, a first sputtering target power supply, a second sputtering target power supply, a third sputtering target power supply, a fourth sputtering target power supply, a first ion source power supply and a first bias power supply, wherein the first molecular pump controller is used for controlling a first molecular pump arranged on the fine pumping system.
2. The multi-target direct current magnetron sputtering apparatus according to claim 1, characterized in that: the rough pumping system comprises a first rotary vane pump, a first roots pump, the first thermocouple vacuum gauge, a fifth valve and a sixth valve.
3. The multi-target direct current magnetron sputtering apparatus according to claim 2, characterized in that: the fine pumping system comprises a second rotary vane pump, a first valve, the first molecular pump, a second valve and a third valve;
the rough pumping system is communicated with the fine pumping system, and a fourth valve is arranged on a communicated pipeline.
4. The multi-target direct current magnetron sputtering apparatus according to claim 3, wherein: the first valve, the second valve, the third valve and the fifth valve are all pneumatic vacuum valves;
the third valve is a pneumatic high valve;
the sixth valve is a pneumatic air release valve.
5. The multi-target direct current magnetron sputtering device according to any one of claims 1 to 4, wherein: the first sputtering target, the second sputtering target, the fourth sputtering target and the fifth sputtering target are cylindrical targets, and the height of the cylindrical targets is 800-1000 mm;
the third sputtering target is a plane target with the height of 600-800 mm.
6. Use of the multi-target dc magnetron sputtering device according to any one of claims 1 to 4 for depositing multiple metal films on a substrate surface.
7. A method for depositing a Ti-Cu-Ti-Au multilayer film on a substrate surface, comprising the steps of:
s1, preprocessing a substrate;
s2, mounting the substrate on the first workpiece frame in the multi-target direct current magnetron sputtering device in any one of claims 1 to 4, and closing a furnace door; starting the rough pumping system and the fine pumping system to perform rough pumping and fine pumping on the coating chamber in sequence, and closing the rough pumping system when the pressure in the coating chamber reaches a preset value;
s3, introducing high-purity argon into the film coating chamber through the first flowmeter; starting the first heating pipe to heat the substrate, and starting the first ion source to perform plasma bombardment cleaning on the surface of the substrate;
s4, turning off the ion source, turning on the first sputtering target power supply and the second sputtering target power supply, and depositing a first layer of Ti on the surface of the substrate by using the first sputtering target and the second sputtering target;
s5, turning off the first sputtering target power supply and the second sputtering target power supply, turning on the fourth sputtering target power supply and the fifth sputtering target power supply, and depositing a second layer of Cu on the surface of the substrate by using the fourth sputtering target and the fifth sputtering target;
s6, turning off the fourth sputtering target power supply and the fifth sputtering target power supply, turning on the first sputtering target power supply and the second sputtering target power supply, and depositing a third layer of Ti on the surface of the substrate by using the first sputtering target and the second sputtering target;
s7, turning off the first sputtering target power supply and the second sputtering target power supply, turning on the third sputtering target power supply, and depositing a fourth layer of Au on the surface of the substrate by using the third sputtering target;
s8, closing the third sputtering target power supply, the first heating pipe, the first bias power supply, the rough pumping system and the fine pumping system, and filling argon for cooling to obtain the Ti-Cu-Ti-Au multilayer film on the substrate.
8. The method of claim 7, wherein: in the step S2, rough pumping and fine pumping are carried out on the coating chamber according to the following steps:
opening the first rotary vane pump and the fifth valve, roughly pumping the film coating chamber until the indication number of the first thermocouple vacuum gauge is less than 5 multiplied by 10 2 When Pa, the first roots pump is started; simultaneously opening the second rotary vane pump, the second valve and the first molecular pump; to be divided intoAfter the sub-pump is started normally and the indication number of the second thermocouple vacuum gauge is less than 1Pa, opening the second valve and carrying out fine pumping on the film coating chamber;
the pressure in the film coating chamber is lower than 8 x 10 -3 And after Pa, closing the fifth valve, the first roots pump and the first rotary vane pump.
9. The method according to claim 7 or 8, characterized in that: in the step S3, the heating temperature is 150-200 ℃ and the time is 60-120 min;
when plasma bombardment cleaning is carried out, the bias voltage is controlled to be 0-200V and 0-99 percent;
in step S4, before deposition, the air exhaust angle of the third valve is adjusted to be 0-90 degrees, the pressure of the film coating chamber is controlled to be 0.1-1 Pa, the bias voltage is controlled to be 0-200V, and the bias voltage is 0-99%.
10. The method according to any one of claims 7-9, wherein: in step S4, the currents of the first sputtering target power supply and the second sputtering target power supply are 10-15A;
the deposition time is 5-20 min, the bias voltage is 0-200V, 0-99%;
in step S5, the currents of the fourth sputtering target power supply and the fifth sputtering target power supply are 10 to 15A;
the deposition time is 30-60 min, the bias voltage is 0-200V, 0-99%;
in step S6, the current of the first sputtering target power supply and the second sputtering target power supply is 10 to 15A;
the deposition time is 5-20 min, the bias voltage is 0-200V, 0-99%;
in step S7, the current of the third sputtering target power supply is 3-5A;
the deposition time is 30-120 min.
11. The method according to any one of claims 7-10, wherein: after the step S8, the method further includes the following step of Au plating:
repeating the step S2, and opening the first heating pipe to preheat the workpiece; introducing high-purity argon, and adjusting the air extraction angle by adjusting the third valve; and repeating the step S7 to perform Au coating.
12. A Ti-Cu-Ti-Au multilayer film prepared by the method of any one of claims 7 to 11.
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