CN113061857A

CN113061857A - Method and equipment for depositing film by ion-assisted, inclined sputtering and reactive sputtering

Info

Publication number: CN113061857A
Application number: CN202110268042.3A
Authority: CN
Inventors: 唐云俊; 王昱翔; 周虹玲; 周东修
Original assignee: Zhejiang Aiweipu Technology Co ltd
Current assignee: Zhejiang Aiweipu Technology Co ltd
Priority date: 2021-03-12
Filing date: 2021-03-12
Publication date: 2021-07-02
Anticipated expiration: 2041-03-12
Also published as: CN113061857B

Abstract

The invention discloses a method for depositing a film by ion-assisted, inclined sputtering and reactive sputtering, which comprises the following steps of debugging operation parameters, compiling a hysteresis loop menu, firstly determining basic parameters, wherein the basic parameters comprise the power of an ion source power supply, the power of a radio frequency power supply connected with a target material, the power of a pulse power supply, the inclination angle of a substrate table, the pressure of process gas, the flow change of the process gas and the process time, then setting the parameters, operating according to the set parameters, finishing the appointed process time, and downloading a substrate.

Description

Method and equipment for depositing film by ion-assisted, inclined sputtering and reactive sputtering

Technical Field

The invention belongs to the field of film physical vapor deposition systems, and particularly relates to an ion-assisted, inclined sputtering and reactive sputtering oxide and nitride, such as Al₂O₃、AlN_xA method of making a thin film.

Background

Oxide, nitride films, e.g. Al₂O₃The film is an important functional film material.

Due to Al₂O₃The film has high dielectric constant, high heat conductivity and strong radiation damage resistance. The material has the advantages of strong alkali ion penetration resistance, transparency in a wide wavelength range and other excellent physical and chemical properties, so that the material has wide application in the fields of microelectronic devices, electroluminescent devices, optical waveguide devices, corrosion-resistant coatings and the like.

Al₂O₃Thin films are widely used in the fabrication of microelectronic devices, one important application being for insulating layers.

Since many different 3D structures are usually present on the substrate surface during the fabrication of electronic devices, this requires deposition of Al₂O₃The film has the advantages of high deposition rate, uniformity of film thickness, high dielectric constant and high coverage rate (conformal) on the 3D structure on the substrate.

Al₂O₃The preparation method of the film has various methods, such as ion-assisted sputtering, radio frequency magnetron sputtering, pulse reaction magnetron sputtering, chemical vapor deposition, atomic layer deposition, sol-gel method and the like.

The film prepared by ion-assisted deposition has the characteristics of high film-substrate bonding strength, high film density and the like, and is widely applied to the preparation of structural film materials and functional film materials, particularly optical film preparation. But the deposition rate is very low, typically less than 0.1 nm/sec.

Radio frequency magnetron sputtering Al₂O₃The rate of the film is very low, in the filmHigh-power operation is needed in the preparation process, so that the temperature of a system cavity is high, particles in the cavity are increased, the technological process is unstable, the temperature of a substrate is high, and the like; and a higher wrapping rate (consistency) of the 3D structure on the substrate cannot be formed.

The pulse reaction magnetron sputtering has high film deposition rate, can keep the uniformity of the film in a large area range, and can effectively solve the problem of preparing Al₂O₃The discharge effect in thin films has become a hot point of research. However, the conventional impulse reactive magnetron sputtering cannot form a high coverage rate (conformal) of the 3D structure on the substrate.

Reactive sputtering, which generally has a "hysteresis loop" effect, i.e., the current or voltage of the target changes with the flow of the reactive gas, resulting in sudden change; and the voltage/current change of the gradually increasing section of the gas flow is not overlapped with the voltage/current change of the gradually decreasing section of the gas flow, so as to form a hysteresis loop, as shown in fig. 1. This is due to the different escape voltages of the sputtered material at different reactant gas flow rates on the surface of the metal target. Under the condition of the reaction gas flow less than the point A, metal materials are mainly sputtered, the target material voltage is higher, the sputtering rate is also high, and the sputtering mode is called as a metal mode; under the condition of the reaction gas flow rate larger than the point B, oxide materials are mainly sputtered, the target material voltage is lower, the sputtering rate is also low, and the sputtering mode is called as a poisoning mode; between points A-B, metal and oxide mixed materials are sputtered, and the material is called as a transition mode; the B-C point area can form a stable oxide film, has a high sputtering rate and is an ideal stable process area.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a reactive sputtering method and equipment adopting ion assistance, inclined sputtering, a mixing power supply and substrate cooling, and overcomes the defects of low deposition rate of the existing alumina film, low coating rate of a 3D structure on a substrate and higher substrate temperature.

In order to achieve the purpose, the invention provides the following technical scheme: a method for depositing film by ion-assisted, inclined sputtering and reactive sputtering comprises the following steps,

s1: debugging the operation parameters, firstly compiling a hysteresis loop menu, uploading a substrate, operating the hysteresis loop menu, drawing and recording a hysteresis loop, determining the numerical value of each parameter during stable reactive sputtering, recording the numerical value as a specified value, and downloading the substrate after debugging is finished;

s2: setting parameters, namely uploading the substrate to a substrate table of the process cavity;

s2.1: rotating the substrate table to a specified inclination angle phi, and then enabling the substrate table to rotate around the center of the substrate at the rotating speed omega;

s2.2: opening a process gas flowmeter, introducing a specified gas flow into a vacuum chamber of a process cavity, and controlling the air pressure p in the vacuum chamber of the process cavity to a specified value;

s2.3: setting a coil current I _ t of the top magnet and a coil current I _ b of the bottom magnet to a specified value to generate a magnetic field to guide plasma;

s2.4: setting the power Pw of an ion source power supply to a specified value so as to generate plasma in a vacuum chamber of the process cavity;

s2.5: setting the radio frequency power supply power Pwr and the pulse power supply power Pwp which are connected with the target to a specified value and frequency f, and setting the inversion time t to the specified value;

s3: and operating according to the set parameters, finishing the appointed process time, and downloading the substrate.

Further, in step S1, when the hysteresis loop menu is compiled, basic parameters including the power of the ion source and the rf power, the power of the pulse power, the tilt angle of the substrate table, the process gas pressure, the process gas flow change, and the process time of the target are determined, and then the hysteresis loop menu is executed.

Further, in step S1, when the hysteresis loop menu is executed, the system records the target current and voltage variation values along with the reactant gas, and simultaneously draws a hysteresis loop, where the point of sudden increase of the target current in the hysteresis loop is the poisoning point, and the corresponding reactant gas Flow is labeled as Flow _ pp.

Further in step S1, a reactive gas Flow value Flow _ stable at the time of stable reactive sputtering is determined (Flow _ pp-Y) < Flow _ stable < Flow _ pp-X,

wherein X is 1-2 sccm; y ═ X + a; and A is 2-3 sccm.

Further, in step S1, after determining the reactive gas flow rate value during stable reactive sputtering, if the basic parameter is to be changed, the hysteresis loop menu is recompiled and then the operation is performed again.

Further, in step S2.1, the inclination angle Φ of the substrate table is 30 to 80 degrees, and the rotation speed ω of the substrate table rotation is 0 to 60 RPM.

Further in step S2.2, the process gas has a flow rate of 0 to 200sccm and the pressure in the vacuum chamber of the process chamber is 1 to 20 mTorr.

Further in step S2.3, the coil current I _ t of the top magnet is 0-200A; the coil current I _ b of the bottom magnet is 0 to 200A.

Further in step S2.4, the ion source power Pw is 0 to 10 kW.

Further in step S2.5, the rf power Pwr of the target is 0-10 kW; the power Pwp of the pulse power supply is 0-10 kW; the frequency f of the pulse power supply is 1-400 kHz; the inversion time t is 0-20 μ sec.

The utility model provides an equipment of supplementary, slope sputtering of ion, reactive sputtering deposit film, includes the technology cavity, is provided with plasma source, target holder and substrate platform in the technology cavity, be provided with the gas around the front of substrate platform and spray the unit, still include substrate conveying vacuum cavity and substrate and upload the cavity, the technology cavity is connected with substrate conveying vacuum cavity, and is provided with first vacuum valve between the two, substrate is uploaded the cavity and is connected with substrate conveying vacuum cavity and is provided with the second vacuum valve between the two, substrate is uploaded the cavity and still is provided with the door that supplies the substrate to put into, be provided with the manipulator in the substrate conveying vacuum cavity.

The gas spraying unit further comprises a plurality of spray holes, the plurality of spray holes are uniformly distributed on the inner side of the gas spraying ring along the circumference, and a gas passage communicated with the spray holes is formed in the gas spraying ring.

Further, a sealing unit is arranged on the front surface of the substrate table, the sealing unit is arranged along the outline shape of the substrate table, the substrate is arranged on the sealing unit, a cavity is formed between the substrate and the substrate table, and a gas channel communicated to the cavity is formed in the substrate table.

Furthermore, a cooling channel is arranged in the substrate table, and a cooling medium is introduced into the cooling channel.

The plasma source is provided with a plasma source, a substrate table, a target support and a substrate table, wherein the plasma source is arranged in a plasma chamber, the target support is positioned below the plasma source, the front surface of the target support is obliquely arranged at an angle with the central axis of the plasma source, and the front surface of the substrate table faces to the front surface of the target support and is far away from the central axis of the plasma source.

Further, a top magnet and/or a bottom magnet is disposed within the chamber, the top magnet being located at the plasma source and the bottom magnet being located at the substrate table.

Further, the top magnet is arranged at an angle of 0-90 degrees with respect to the central axis of the plasma source, and the bottom magnet is arranged at an angle of 0-90 degrees with respect to the central axis of the substrate table.

Compared with the prior art, the invention has the beneficial effects that: overcoming the existing oxide and nitride films, such as Al₂O₃The method has the defects of low film deposition rate, low coating rate on the 3D structure on the substrate and high substrate temperature, and can realize Al₂O₃Film deposition rate>1 nm/sec; coating rate of 3D structure>50 percent; substrate temperature<50℃。

Drawings

FIG. 1 is a schematic diagram of a hysteresis loop in the prior art;

FIG. 2 is a schematic structural view of a process chamber according to the present invention;

FIG. 3 is a schematic perspective view of a gas spray unit in the reactive sputtering apparatus;

FIG. 4 is a cross-sectional view of a gas spray unit in the reactive sputtering apparatus;

FIG. 5 is a schematic view of a substrate table having a baffle plate;

FIG. 6 is a cross-sectional view of a substrate table;

FIG. 7 is an overall view of an apparatus for ion-assisted, tilted sputtering, reactive sputtering deposition of thin films in accordance with the present invention;

FIG. 8 is a schematic diagram of a hysteresis loop of the present invention;

FIG. 9 is a photograph of an FIB under process conditions according to one embodiment.

Reference numerals: 10. a process chamber; 101. a first vacuum valve; 11. a substrate transfer vacuum chamber; 111. a manipulator; 112. a second vacuum valve; 12. a substrate uploading cavity; 2. a plasma source; 3. a target holder; 4. a substrate stage; 42. a baffle plate; 43. a shaft; 45. an air injection ring; 51. a top magnet; 52. a bottom magnet; 6. a substrate; 71. spraying a hole; 73. an airway; 81. a seal ring; 82. a gas channel; 83. a cavity; 84. a vacuum pump; 85. a capacitance manometer; 86. a controller; 87. a valve; 88. a mass flow controller; 89. a cooling channel.

Detailed Description

In the description of the present invention, it should be noted that, for the terms of orientation, such as "central", "lateral (X)", "longitudinal (Y)", "vertical (Z)", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc., indicate that the orientation and positional relationship are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and should not be construed as limiting the specific scope of the present invention.

Furthermore, if the terms "first" and "second" are used for descriptive purposes only, they are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features. Thus, a definition of "a first" or "a second" feature may explicitly or implicitly include one or more of the features, and in the description of the invention, "a number" or "a number" means two or more unless explicitly specified otherwise.

Ion-assisted, tilted sputtering, reactive sputtering of oxide, nitride films, e.g. Al₂O₃、AlN_xThe apparatus for thin film deposition also includes a substrate 6 loading chamber 12(LL), as shown in FIG. 7. The substrate 6 loading chamber 12 is provided with a door, and when opened, a cassette of substrates 6 carrying the substrates 6 can be placed therein. A second vacuum valve 87112 is arranged between the substrate 6 loading chamber 12 and the substrate 6 transferring vacuum chamber 83 and the body 11. LL is pumped to vacuum by vacuum pump 84.

Ion-assisted, tilted sputtering, reactive sputtering of oxide, nitride films, e.g. Al₂O₃The apparatus for thin film deposition also includes a vacuum chamber 83 for transporting the substrate 6 (TM) and a vacuum chamber 11(TM), as shown in FIG. 7. The substrate 6 transfer vacuum chamber 83 is provided with a robot 111 in the body 11. A second vacuum valve 87112 is arranged between the conveying vacuum cavity 83 and the process cavity 10, and a first vacuum valve 87101 is arranged between the conveying vacuum cavity 83 11 of the substrate 6 and the upper loading cavity 12 of the substrate 6. The robot 111 in the substrate 6 transfer vacuum chamber 83 body 11 can grasp a given substrate 6 from the substrate 6 upper load chamber 12 into the substrate 6 transfer vacuum chamber 83 body 11 while the second vacuum valve 87112 between the substrate 6 transfer vacuum chamber 83 body 11 and the substrate 6 upper load chamber 12 is opened, and thereafter the second vacuum valve 87112 is closed. The robot 111 then transfers the substrate 6 to the substrate stage 4 of the process chamber 10 while the first vacuum valve 87101 between the transfer vacuum chamber 83 and the process chamber 10 is opened, thereby completing the process of loading the substrate 6.

Ion-assisted, tilted sputtering, reactive sputtering of oxide, nitride films, e.g. Al₂O₃、AlN_xThe thin film deposition apparatus includes a process chamber 10, as shown in fig. 2. A plasma source 2, a target support 3 and a substrate table 4 are arranged in the process cavity 10, and a gas spraying unit is arranged around the front face of the substrate table 4.

The preferred gas spraying unit of this embodiment includes the gas injection ring 45, and the substrate table 4 is used for placing the substrate 6 in the middle of corresponding gas injection ring 45, the gas spraying unit also includes a plurality of spray orifices 71, and a plurality of spray orifices 71 are evenly distributed along the circumference at the inboard of gas injection ring 45, be provided with the air flue 73 with spray orifice 71 intercommunication on the gas injection ring 45.

One end of the air channel 73 is a gas inlet which is connected with a gas source.

In this embodiment, in order to make the gas flow ejected from all the nozzle holes 71 uniform, it is preferable that the path distances of the gas passages 73 from the inlets of the gas passages 73 to all the nozzle holes 71 are the same, and a multi-stage channel form may be adopted, each channel is divided into two branches as a next-stage channel, the path distances of the two branches of the same stage are the same, and the last-stage channel forms the nozzle holes 71.

In the preferred embodiment, an openable baffle 42 is disposed in front of the substrate table 4, the baffle 42 in the preferred embodiment is rotatably connected to the plate on the substrate table 4 via a shaft 43, and preferably driven by a motor, the baffle 42 can rotate around the shaft 43, so that it covers or uncovers the substrate 6 on the substrate table 4, although the baffle 42 can also cover or uncover the substrate 6 in a translational manner.

In the preferred embodiment, a sealing unit is disposed on the front surface of the substrate stage 4, the sealing unit is disposed along the contour of the substrate stage 4, the substrate 6 is disposed on the sealing unit, the sealing unit can be, for example, a sealing ring 81, a cavity 83 is formed between the substrate 6 and the substrate stage 4, a gas passage 82 communicated with the cavity 83 is opened on the substrate stage 4, the substrate 6 can be attached to the sealing unit by connecting the gas passage 82 to a vacuum pump 84, and the substrate stage 4 can be manufactured simply.

A capacitance manometer 85 for measuring a flow rate of gas drawn from the cavity 83 may be provided between the gas passage 82 and the vacuum pump 84, and a controller 86 for cooperating with the capacitance manometer 85 may be further included, the controller 86 controlling the flow rate of the drawn gas to thereby control the pressure of the gas in the cavity 83.

Preferably, a branch between the gas channel 82 and the capacitance manometer 85 is provided, which is provided with a valve 87 and a mass flow controller 88, and the gas in the cavity 83 can be introduced into the cavity 83 by opening the valve 87, and the constant pressure of the gas in the cavity 83 is controlled by the valve 87, the mass flow controller 88, the capacitance manometer 85, the controller 86 and the vacuum pump 84 together during the deposition process.

During deposition, the gas in the cavity 83 may act as a thermal conductor between the substrate 6 and the substrate table 4, so that the substrate 6 and the substrate table 4 are thermally conductive.

In the preferred embodiment, a cooling channel 89 is formed in the substrate stage 4, a cooling medium is introduced into the cooling channel 89, and water or a water-alcohol mixture, for example, is introduced into the cooling channel 89 as a cooling medium to flow through the substrate stage 4, so as to accelerate heat dissipation.

The preferred target holder 3 of this embodiment is located below the plasma source 2, and the front face of the target holder 3 is arranged obliquely at an angle to the central axis 43 of the plasma source 2, and the front face of the substrate stage 4 faces the front face of the target holder 3 and is away from the central axis 43 of the plasma source 2.

Wherein the preferred substrate table 4 may employ a rotation mechanism to enable in-situ rotation of the substrate 6 about the axis 43.

Of course, the substrate stage 4 as a whole can be rotated relative to the target holder 3 to adjust the angle between it and the target holder 3.

The central axis 43 of the plasma source 2 is the plasma path in this embodiment, and the substrate table 4 keeps the substrate away from the plasma path, but directs the substrate towards the sputtering surface of the target on the target holder 3 to maximize deposition of sputtered material on the substrate.

The target holder 3 in this embodiment preferably can rotate the target material by using a rotating mechanism, but the inclination angle of the target holder 3 is preferably adjustable, but these are not essential.

In the preferred embodiment, a top magnet 51 and/or a bottom magnet 52 are disposed in the chamber, wherein the top magnet 51 is located at the plasma source 2 and the bottom magnet 52 is located at the substrate stage 4.

The preferred embodiment of the top magnet 51 is disposed at an angle of 0-90 deg. to the axis 43 of the plasma source 2.

The preferred embodiment of the bottom magnet 52 is disposed at an angle of 0-90 deg. to the centerline of the substrate table 4.

The two magnets may be electromagnetic coils or ring magnets. The top and

bottom magnets

51, 52 may generate magnetic fields with asymmetric strengths, thereby forming magnetic field lines that may be manipulated to control the concentration of ions emitted by the plasma source 2 and reaching the target.

Ion-assisted, tilted sputtering, reactive sputtering of oxide, nitride films, e.g. Al₂O₃、AlN_xThe film deposition method comprises the following steps:

s1: debugging the operation parameters, firstly compiling a hysteresis loop menu, uploading the substrate 6, operating the hysteresis loop menu, drawing and recording a hysteresis loop, determining the numerical value of each parameter during stable reactive sputtering, recording the numerical value as a specified value, and downloading the substrate 6 after debugging is finished;

s2: setting parameters, namely uploading a substrate 6 onto a substrate table 4 of a process cavity 10;

s2.1: rotating the substrate table 4 to a specified inclination angle phi, and then enabling the substrate table 4 to rotate around the center of the substrate 6 at the rotating speed omega;

s2.2: opening a process gas flowmeter, introducing a specified gas flow into a vacuum cavity 83 of the process chamber 10, and controlling the pressure p in the vacuum cavity 83 of the process chamber 10 to a specified value;

s2.3: setting the coil current I _ t of the top magnet 51 and the coil current I _ b of the bottom magnet 52 to specified values to generate a magnetic field to guide plasma;

s2.4: setting the ion source power Pw to a specified value to generate a plasma in the vacuum chamber 83 of the process chamber 10;

s3: and operating according to the set parameters to finish the appointed process time, and downloading the substrate 6.

In step S1, preferably, when the hysteresis loop menu is compiled, the basic parameters, the power of the ion source power source, the power of the rf power source connected to the target, the power of the pulse power source, the tilt angle of the substrate stage 4, the process gases (Ar, O), and the like, are determined first₂、N₂) The pressure of (a); flow of process gases, e.g. Ar, O₂、N₂A change in gas flow rate; and (5) the process time is shortened, and then the hysteresis loop menu is operated. The process gas in this embodiment includes Ar, O₂、N₂。

In step S1, the system preferably records the target current and voltage along with the reaction gas (O) while running the hysteresis loop menu₂、N₂) The flow change value is drawn, a delay loop is drawn at the same time, and the point of the sudden increase of the target current in the delay loop is the poisoning point corresponding to the reaction gas (O)₂、N₂) The Flow is labeled Flow _ pp. The reaction gas in this embodiment is a gas involved in the reaction of the process gas, and includes O₂、N_2。

In step S1, the reactive gas such as O during stable reactive sputtering is determined₂，N₂Flow value of gas Flow _ stable:

(Flow_pp-Y)<Flow_stable<Flow_pp-X，

wherein X is 1-2 sccm; y ═ X + a; and A is 2-3 sccm.

As shown in FIG. 8 and Table 1, under the condition that Flow _ pp was measured to be 36sccm, O was taken according to the above formula₂The stable film thickness and refractive index can be obtained by respectively operating the thin film deposition processes at the flow rates of 33.8, 34.2, 34.4, 34.6 and 34.8sccm, which indicates that the stable thin film deposition process is formed in this interval, i.e., indicates that the process S1 is completed.

Table 1:

this embodiment is preferable in step S1, when stable reactive sputtering is determined, the reactive gas, such as O₂、N₂After the flow value is obtained, if the basic parameters need to be changed, the hysteresis loop menu is recompiled and then the operation is carried out again.

As shown in table 2, which are several cases of the specific implementation of the process run S2 procedure.

Table 2:

B	C	D	E	F	G	H	I	G	L	M
											Deg	w	w	w	mTorr	sccm	sccm	sec	nm	％	nm/sec
75	3500	3200	1000	3	90	29.4	1000	1042.8	0.63	1.043
											65	3500	3200	1000	3	90	29.4	1040	1034.9	0.58	0.995
55	3500	3200	1000	3	90	29.0	1155	1053.9	0.57	0.912
											45	3500	3200	1000	3	90	28.8	1320	1032.7	0.50	0.785
35	3500	3200	1000	3	90	28.6	1575	1045.7	0.25	0.664
											25	3500	3200	1000	3	90	28.0	2200	1060.0	0.75	0.482

in Table 2, B is the tilt angle of the substrate table 4; c is the power of the ion source power supply; d is the radio frequency power supply power connected with the target material; e is the power of the pulse power supply; f is process gas Ar and O₂The pressure of (a); g is Ar flow; h is O₂Flow rate; i is deposition time; g is the thickness of the coating film; l is the mean square error σ% of the film thickness; m is the deposition rate.

The basic parameter of the process, namely the inclination angle of the substrate table 4, is changed from 25 degrees to 75 degrees, the inclination angle of each substrate table 4 needs to execute a process debugging process S1, and the corresponding stable process O is obtained₂Flow rate, e.g. when the substrate table 4 is tilted at an angle of 25 degrees, O stabilizing the process₂The flow rate was 28.0 sccm. H value (O) in Table 2₂Flow rates) are respectively O of the stabilization process corresponding to the B value (the inclination angle of the substrate stage 4) measured through the process of S1₂And (4) flow rate.

In step S2.1, the inclination angle Φ of the substrate stage 4 is 30 to 80 degrees, and the rotation speed ω of the substrate stage 4 rotating on its axis is 0 to 60 RPM; in step S2.2, process gases, e.g. Ar, O₂、N₂The flow rate of the PM is 0-200sccm, and the air pressure P in the PM cavity is 1-20 mTorr; in step S2.3, the coil current I _ t of the top magnet 51 is 0-200A; the coil current I _ b of the bottom magnet 52 is 0 to 200A; in step S2.4, the ion source power Pw is 0 to 10 kW; in step S2.5, the rf power Pwr connected to the target is 0-10 kW; the power Pwp of the pulse power supply is 0-10 kW; the frequency f of the pulse power supply is 1-400 kHz; the inversion time t is 0-20 μ sec.

In a certain implementation and operation process case, the inclination angle phi of the substrate table 4 is 75 degrees, and the rotation speed omega of the substrate table 4 is 30 RPM; in step S2.2, the flow rate of Ar is 90 sccm; o is₂The flow rate of (2) is 29.4 sccm; the air pressure P in the process chamber 10 is 3 mTorr; in step S2.3, the coil current I _ t of the top magnet 51 is 100A; the coil current I _ b of the bottom magnet 52 is 190A; in step S2.4, the ion source power Pw is 3.5 kW; in step S2.5, the rf power Pwr of the target is 3.2 kW; the power Pwp of the pulse power supply is 1 kW; frequency f is 40 kHz; the inversion time t is 10 μ sec. The thickness uniformity of the film obtained by the process is the mean square of the thicknessThe difference was 0.63%, and the deposition rate was 1.043 nm/sec.

In another embodiment, the inclination angle phi of the substrate table 4 is 45 degrees, and the rotation speed omega of the substrate table 4 is 30 RPM; in step S2.2, the flow rate of Ar is 90 sccm; o is₂The flow rate of (2) is 29.4 sccm; the air pressure P in the process chamber 10 is 3 mTorr; in step S2.3, the coil current I _ t of the top magnet 51 is 100A; the coil current I _ b of the bottom magnet 52 is 190A; in step S2.4, the ion source power Pw is 3.5 kW; in step S2.5, the rf power Pwr of the target is 3.2 kW; the power Pwp of the pulse power supply is 1 kW; frequency f is 40 kHz; the inversion time t is 10 μ sec. The process was run to obtain a film thickness uniformity of 0.50% thickness mean square error and a deposition rate of 0.785 nm/sec.

As can be seen from table 2, the uniformity of the thickness of the obtained film can meet the requirement of high-precision film deposition (the mean square deviation of the thickness is required to be less than 1.0%); meanwhile, the deposition rate is proportional to the inclination angle of the substrate stage 4, i.e., the higher the inclination angle of the substrate stage 4, the larger the deposition rate.

In another embodiment, the inclination angle phi of the substrate table 4 is 45 degrees, and the rotation speed omega of the substrate table 4 is 30 RPM; in step S2.2, the flow rate of Ar is 90 sccm; o is₂The flow rate of (2) is 29.4 sccm; the air pressure P in the process chamber 10 is 3 mTorr; in step S2.3, the coil current I _ t of the top magnet 51 is 100A; the coil current I _ b of the bottom magnet 52 is 190A; in step S2.4, the ion source power Pw is 3.5 kW; in step S2.5, the rf power Pwr of the target is 3.2 kW; the power Pwp of the pulse power supply is 1 kW; frequency f is 40 kHz; the inversion time t is 10 μ sec. The thickness uniformity of the film obtained by the operation of the process is that the thickness mean square deviation is 0.50 percent, and the deposition rate is 0.785 nm/sec; FIG. 9 also shows the FIB (focused Ion Beam) photograph under the process conditions, and it can be seen that the coverage (coherence) of the 3D structure achieved by the process is t₀50% of t, wherein t₀Is the thickness of the film deposited on the surface of the 3D structure, and t is the thickness of the film deposited on the side surface of the 3D structure.

In a certain process case, the inclination angle phi of the substrate table 4 is 75 degrees, the rotation speed omega of the substrate table 4 is equal to 30 RPM; in step S2.2, the flow rate of Ar is 90 sccm; o is₂The flow rate of (2) is 29.4 sccm; the air pressure P in the process chamber 10 is 3 mTorr; in step S2.3, the coil current I _ t of the top magnet 51 is 100A; the coil current I _ b of the bottom magnet 52 is 190A; in step S2.4, the ion source power Pw is 3.5 kW; in step S2.5, the rf power Pwr of the target is 3.2 kW; the power Pwp of the pulse power supply is 1 kW; frequency f is 40 kHz; the inversion time t is 10 μ sec. The thickness of the film obtained by the operation of the process was about 500nm, the thickness uniformity was such that the mean square deviation of the thickness was 0.63%, the deposition rate was 1.043nm/sec, and the surface temperature of the substrate 6 was measured by using a temperature spot plate at the same time<48 ℃ as shown in Table 3.

In another embodiment, the inclination angle Φ of the substrate stage 4 is 75 °, and the rotation speed ω of the substrate stage 4 is 30 RPM; in step S2.2, Ar and O₂The flow rate of (2) is 90 sccm; o is₂The flow rate of (2) is 29.4 sccm; the air pressure P in the PM cavity is 3 mTorr; in step S2.3, the coil current I _ t of the top magnet 51 is 100A; the coil current I _ b of the bottom magnet 52 is 190A; in step S2.4, the ion source power Pw is 3.5 kW; in step S2.5, the rf power Pwr of the target is 3.2 kW; the power Pwp of the pulse power supply is 1 kW; frequency f is 40 kHz; the inversion time t is 10 μ sec. The thickness of the film obtained by the operation of the process is about 2um, the thickness uniformity is that the mean square deviation of the thickness is 0.63 percent, the deposition rate is 1.043nm/sec, and simultaneously, the surface temperature of the substrate 6 is measured by using a temperature spot plate<48 ℃ as shown in Table 3.

Table 3:

it should be noted that different substrate stage 4 tilt angle processes can be used in different applications to suit specific film deposition process requirements. In general, the smaller the tilt angle of the substrate table 4, the larger the wrap rate of the 3D structure, but the smaller the deposition rate.

The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.

Claims

1. A method for depositing a film by ion-assisted, inclined sputtering and reactive sputtering is characterized by comprising the following steps,

2. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 1, wherein: in step S1, when the hysteresis loop menu is compiled, first, basic parameters are determined, where the basic parameters include power of the ion source and rf power, power of the pulse power, substrate stage tilt angle, process gas pressure, process gas flow change, and process time of the target, and then the hysteresis loop menu is run.

3. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 2, wherein: in step S1, when the hysteresis loop menu is run, the system records the target current and voltage variation values along with the reactant gas, and simultaneously draws a hysteresis loop, where the point of sudden increase of the target current in the hysteresis loop is the poisoning point, and the corresponding reactant gas Flow is labeled as Flow _ pp.

4. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 3, wherein: in step S1, the reactive gas Flow value Flow _ stable at the time of stable reactive sputtering is determined:

(Flow_pp-Y)<Flow_stable<Flow_pp-X，

wherein X is 1-2 sccm; y ═ X + a; and A is 2-3 sccm.

5. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 4, wherein: in step S1, after the reaction gas flow rate value during stable reactive sputtering is determined, if the basic parameter is to be changed, the hysteresis loop menu is recompiled and the operation is resumed.

6. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 5, wherein: in step S2.1, the inclination angle of the substrate table is 30 to 80 degrees, and the rotation speed ω of the substrate table is 0 to 60 RPM.

7. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 6, wherein: in step S2.2, the process gas has a flow rate of 0 to 200sccm and the pressure in the vacuum chamber of the process chamber is 1 to 20 mTorr.

8. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 7, wherein: in step S2.3, the coil current I _ t of the top magnet is 0-200A; the coil current I _ b of the bottom magnet is 0 to 200A.

9. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 8, wherein: in step S2.4, the ion source power Pw is 0 to 10 kW.

10. The method of ion assisted, tilted sputtering, reactive sputtering deposition of thin films as claimed in claim 9, wherein: in step S2.5, the rf power Pwr connected to the target is 0-10 kW; the power Pwp of the pulse power supply is 0-10 kW; the frequency f of the pulse power supply is 1-400 kHz; the inversion time t is 0-20 μ sec.

11. The utility model provides an equipment of supplementary, slope sputtering of ion, reactive sputtering deposition film, includes the technology cavity, is provided with plasma source, target holder and substrate platform in the technology cavity, the positive of substrate platform is provided with gas around spraying the unit, its characterized in that: the vacuum substrate processing device is characterized by further comprising a substrate conveying vacuum cavity and a substrate uploading cavity, the process cavity is connected with the substrate conveying vacuum cavity, a first vacuum valve is arranged between the process cavity and the substrate conveying vacuum cavity, the substrate uploading cavity is connected with the substrate conveying vacuum cavity, a second vacuum valve is arranged between the substrate uploading cavity and the substrate conveying vacuum cavity, the substrate uploading cavity is further provided with a door for placing a substrate, and a manipulator is arranged in the substrate conveying vacuum cavity.

12. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 11, wherein: the gas spraying unit comprises a gas spraying ring, a substrate table corresponds to the middle of the gas spraying ring and is used for placing a substrate, the gas spraying unit further comprises a plurality of spray holes, the plurality of spray holes are evenly distributed on the inner side of the gas spraying ring along the circumference, and a gas passage communicated with the spray holes is formed in the gas spraying ring.

13. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 12, wherein: the surface in front of the substrate platform is provided with a sealing unit, the sealing unit is arranged along the outline shape of the substrate platform, the substrate is arranged on the sealing unit, a cavity is formed between the substrate and the substrate platform, and a gas channel communicated to the cavity is formed in the substrate platform.

14. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 13, wherein: and a cooling channel is arranged in the substrate table, and a refrigerant is introduced into the cooling channel.

15. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 14, wherein: the target support is positioned below the plasma source, the front surface of the target support is obliquely arranged at an angle with the central axis of the plasma source, and the front surface of the substrate table faces the front surface of the target support and is far away from the central axis of the plasma source.

16. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 15, wherein: a top magnet and/or a bottom magnet are disposed within the chamber, the top magnet located at the plasma source and the bottom magnet located at the substrate table.

17. The apparatus for ion assisted, tilted sputter, reactive sputter deposition of thin films as claimed in claim 16, wherein: the top magnet is arranged at an angle of 0-90 degrees with the central axis of the plasma source, and the bottom magnet is arranged at an angle of 0-90 degrees with the central line of the substrate table.