WO2023005677A1 - 制备金属薄膜的物理气相沉积方法 - Google Patents

制备金属薄膜的物理气相沉积方法 Download PDF

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WO2023005677A1
WO2023005677A1 PCT/CN2022/105641 CN2022105641W WO2023005677A1 WO 2023005677 A1 WO2023005677 A1 WO 2023005677A1 CN 2022105641 W CN2022105641 W CN 2022105641W WO 2023005677 A1 WO2023005677 A1 WO 2023005677A1
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film
target
metal
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thin film
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French (fr)
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郭宏瑞
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Beijing Naura Microelectronics Equipment Co Ltd
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Beijing Naura Microelectronics Equipment Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—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
    • C23C14/345—Applying energy to the substrate during sputtering using substrate bias
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—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
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—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

Definitions

  • the invention relates to the technical field of semiconductors, in particular to a physical vapor deposition method for preparing metal thin films.
  • DRAM Dynamic Random Access Memory
  • DRAM cells operate in an array of columns (bit lines, Bit lines) and rows (word lines, Word lines).
  • the bit lines transfer charge between the sense amplifiers to program (write) or acquire (read) the data for a particular cell.
  • the speed at which data can be written to or read from a DRAM cell depends on the resistance of the bit line; the lower the resistance, the faster the data transfer.
  • the resistance of a conductor depends on the scattering points that electrons encounter as they travel along the line. Impurities in the film, grain boundaries, and device surface roughness can slow down the movement of electrons, and the degree to which these factors affect the movement speed is related to the thickness of the film.
  • RC hysteresis resistance-capacitance delay
  • DRAM dynamic random access memory
  • PVD Physical Vapor Deposition
  • the purpose of the present invention is to propose a physical vapor deposition method for preparing a metal thin film, which can increase the binding force of the film base, prevent the metal film from peeling off, and has high density, good crystallization and low resistivity.
  • the invention provides a physical vapor deposition method for preparing a metal thin film, comprising:
  • Step 1 Put the substrate of the film to be deposited on the base of the reaction chamber;
  • Step 2 Introduce the first mixed gas including nitrogen and krypton into the reaction chamber, apply DC power to the target, make the first mixed gas form plasma and bombard the target, so that the A metal nitride film is formed on the substrate;
  • Step 3 stop feeding the first mixed gas into the reaction chamber, feed a second mixed gas including argon and krypton into the reaction chamber, apply DC power to the target, and Applying a bias radio frequency power to the susceptor, applying the DC power can cause the second mixed gas to form plasma and bombard the target, so as to form a metal film on the metal nitride film; applying the radio frequency The power can make the plasma bombard the surface of the metal film to increase the density of the metal film.
  • the step 2 further includes: applying a bias radio frequency power in a first preset range to the susceptor and maintaining it for a first preset time period, so as to perform etching pretreatment on the surface of the substrate.
  • the step 2 includes:
  • the seat applies the bias radio frequency power in the first preset range, and maintains the first preset time length, so as to perform etching pretreatment on the surface of the substrate;
  • the step 3 includes:
  • the flow rate of the argon gas is less than or equal to 100 sccm, and the flow rate of the krypton gas is less than or equal to 50 sccm.
  • the flow rate ratio of the argon gas to the krypton gas is less than or equal to 0.45.
  • the ratio of the flow rate of the krypton gas to the nitrogen gas is greater than or equal to 0.15.
  • the flow rate of the krypton gas is less than or equal to 50 sccm, and the flow rate of the argon gas is less than or equal to 200 sccm.
  • the DC power applied to the target is less than or equal to 20000W.
  • the process conditions in step 1 are: the vacuum degree of the reaction chamber is less than 5 ⁇ 10 -6 Torr; the temperature of the susceptor is greater than or equal to 250°C and less than or equal to 350°C.
  • a metal nitride thin film is first formed on the surface of the substrate through step 2.
  • the metal nitride thin film can not only increase the film-base bonding force between the subsequently deposited metal thin film and the substrate, and avoid Depositing the metal film directly on the substrate causes lattice mismatch, causing the metal film to peel off, and can also make the subsequently formed metal film grow preferentially along the [110] crystal direction.
  • the interdiffusion phenomenon of the substrate can act as a barrier layer to ensure the low resistance characteristics of the metal film, maintain the stability of device performance and ensure the yield.
  • step 2 adopts the first mixed gas of nitrogen and krypton (Kr) to form plasma, relative to the Ar gas in the prior art, the mass of Kr ion is bigger, because the mass is bigger, the kinetic energy is bigger, this makes After the target is bombarded by Kr ions, the energy of atoms sputtered out and deposited on the substrate is greater, which can change the disordered arrangement of low-energy atoms on the surface of the substrate and improve the migration and diffusion of atoms on the surface of the film, thereby improving Thin film density, crystalline quality, and increasing the atomic energy can also make the crystal grains grow continuously, reducing the barrier effect of electrons crossing the grain boundary, thereby significantly reducing the resistivity of the film and improving the conductivity.
  • Kr krypton
  • step 3 by mixing nitrogen and krypton, not only can the ratio of the two be adjusted to reduce the film resistivity, improve process stability and flexibility, but also reduce the cost of use.
  • step 3 by applying biased radio frequency power to the susceptor, the plasma can be bombarded on the surface of the metal film to increase the density of the metal film and promote the deposition of a high-quality, low-resistivity metal film.
  • FIG. 1 shows a flowchart of a method for preparing a metal thin film by physical vapor deposition according to an embodiment of the present invention.
  • FIG. 2 shows the comparison of the resistivity of the metal thin film formed by the method of the prior art and the method of an embodiment of the present invention.
  • FIG. 3 shows the square resistance and its uniformity distribution diagram of the metal thin film according to an embodiment of the present invention.
  • FIG. 4 shows a crystal XRD pattern of a metal thin film according to an embodiment of the present invention.
  • connection should be understood in a broad sense, for example, it can be a fixed connection or a detachable connection. Connected, or integrally connected; it may be mechanically connected, may be directly connected, or may be indirectly connected through an intermediary. Those of ordinary skill in the art can understand the specific meanings of the above terms in the present invention in specific situations.
  • Fig. 1 shows a flow chart of a physical vapor deposition method for preparing a metal thin film according to an embodiment of the present invention, please refer to Fig. 1, the method includes the following steps:
  • Step 1 Put the substrate of the film to be deposited on the base of the reaction chamber;
  • Step 2 Introducing the first mixed gas comprising nitrogen and krypton into the reaction chamber, applying DC power to the target, so that the first mixed gas forms plasma and bombards the target to form a metal nitride film on the substrate;
  • Step 3 stop feeding the first mixed gas into the reaction chamber, feed the second mixed gas including argon and krypton into the reaction chamber, apply DC power to the target, and apply bias RF power to the base, Applying the above-mentioned DC power can make the second mixed gas form plasma and bombard the target to form a metal film on the metal nitride film; applying the above-mentioned radio frequency power can make the plasma bombard the surface of the metal film to improve the metal film. Density.
  • the preparation of the thin film is carried out in the reaction chamber of the semiconductor equipment.
  • the reaction chamber is provided with a base for carrying the substrate of the thin film to be deposited.
  • the base may have a heating or cooling function.
  • the reaction chamber is connected with a vacuum system, which can pump air to the reaction chamber to make the reaction chamber reach a higher vacuum degree to meet the vacuum conditions required by the process.
  • the gas required for the process is connected to the reaction chamber through a flow meter, and the target required for the process is sealed in the upper area of the reaction chamber.
  • the target material for depositing metal thin film can be pure metal or metal compound.
  • the excitation power supply will apply excitation power (such as DC power, RF power or a combination of the two) to the target, making it negatively biased relative to the grounded reaction chamber, combined with the high voltage in the chamber to ionize and discharge the gas Instead, a positively charged plasma is generated, which is attracted to and bombards the target.
  • excitation power such as DC power, RF power or a combination of the two
  • a positively charged plasma is generated, which is attracted to and bombards the target.
  • the energy of the plasma is high enough, the atoms on the surface of the target will escape and be deposited on the substrate to achieve thin film deposition on the surface of the substrate.
  • This embodiment takes depositing a molybdenum (Mo) thin film on the surface of a substrate as an example to describe in detail the physical vapor deposition method for preparing a metal thin film provided in the embodiment of the present invention.
  • Mo molybdenum
  • step 1 is performed.
  • suitable process conditions are set for the reaction chamber, the substrate of the film to be deposited is placed on the base of the reaction chamber, and the temperature of the base is adjusted to the temperature required by the process. temperature.
  • the substrate is silicon oxide for depositing a molybdenum film
  • the set process conditions are that the vacuum degree of the reaction chamber is less than 5 ⁇ 10 -6 Torr; the temperature of the susceptor is greater than or equal to 250°C , and less than or equal to 350°C, preferably, the temperature of the base is 300°C.
  • a metal Mo target with a purity ⁇ 99.999wt% can be used, and the impurity oxygen (O) content of the metal Mo target is ⁇ 100 wtppm.
  • Execute step 2 feed the first mixed gas including nitrogen and krypton into the reaction chamber, apply DC power to the target (Mo), make the first mixed gas form plasma and bombard the target, so as to form nitrogen on the substrate Molybdenum thin film.
  • target Mo
  • Execute step 2 feed the first mixed gas including nitrogen and krypton into the reaction chamber, apply DC power to the target (Mo), make the first mixed gas form plasma and bombard the target, so as to form nitrogen on the substrate Molybdenum thin film.
  • the sputtering gas is argon (Ar).
  • Ar argon
  • the ions collide, scatter, and partly dissipate to the surface of the substrate, where a Mo film is deposited on the surface of the substrate.
  • the Mo atoms sputtered out by Ar ions bombarding the target and deposited on the substrate have low energy and are arranged in a disordered state, resulting in a loose and not dense film, and a strong barrier effect when electrons cross the grain boundary, resulting in The resistivity of the Mo film is too high, which cannot meet the technological requirements of the advanced manufacturing process.
  • the existing technology is to directly sputter the Mo thin film on the substrate, which will lead to a large stress of the Mo thin film and poor bonding force of the film base, which is easy to peel off.
  • a molybdenum nitride film is formed on the surface of the substrate.
  • Depositing a Mo film on the substrate causes lattice mismatch, causing the Mo film to peel off, and can also make the subsequently formed Mo film grow preferentially along the [110] crystal direction.
  • the interdiffusion phenomenon which can act as a barrier layer, ensures the low resistance characteristics of the Mo film, maintains the stability of device performance and ensures the yield.
  • the preparation of above-mentioned molybdenum nitride film adopts the first mixed gas of nitrogen and krypton (Kr) to form plasma, relative to the Ar gas in the prior art, the quality of Kr ion is bigger, because the mass is bigger, the kinetic energy is higher Larger, which makes the energy of Mo atoms sputtered out of the target and deposited on the substrate after being bombarded by Kr ions is greater, which can change the disordered arrangement of low-energy Mo atoms on the substrate surface and improve the migration of Mo atoms on the film surface And diffusion ability, which can improve the density and crystal quality of the film, and increasing the energy of Mo atoms can also make the grain grow continuously, reduce the potential barrier effect of electrons crossing the grain boundary, thereby significantly reducing the resistivity of the film and improving the electrical conductivity. sex.
  • Execute step 3 stop feeding the first mixed gas into the reaction chamber, feed the second mixed gas including argon and krypton into the reaction chamber, apply DC power to the target, and apply bias RF power to the base , applying DC power can make the second mixed gas form plasma and bombard the target to form a Mo film on the molybdenum nitride film; applying radio frequency power can make the plasma bombard the surface of the Mo film to improve the induction of the Mo film density.
  • the preparation of the above-mentioned Mo thin film adopts the second mixed gas of argon and krypton (Kr) to form plasma, which can also improve the film density and crystallization quality, and can significantly reduce the resistivity of the film, improve conductivity.
  • Kr argon and krypton
  • step 2 by applying bias radio frequency power to the susceptor, a certain bombardment etching can be carried out to the formed molybdenum nitride thin film and the surface of the formed Mo thin film (etching speed is less than the deposition speed), and the etching effect can be Reduce the surface defects of the film while reducing the surface roughness of the film to increase the density of the metal film and promote the deposition of high-quality, high-density low-resistivity Mo film.
  • step 2 optionally, the process pressure of the reaction chamber is maintained at a range greater than or equal to 10 mTorr and less than or equal to 25 mTorr, and the flow range of krypton (Kr) is less than or equal to 50 sccm, preferably Less than or equal to 10 sccm; the flow range of nitrogen is less than or equal to 200 sccm, preferably greater than or equal to 10 sccm, and less than or equal to 80 sccm.
  • Kr krypton
  • the ratio of nitrogen gas is too low, it is easy to form a metastable MoN film, and it is difficult to maintain process stability. This problem can be avoided by making the ratio of krypton gas to nitrogen gas greater than or equal to 0.15.
  • the thickness of the formed molybdenum nitride film is greater than or equal to 20 angstroms and less than or equal to 60 angstroms.
  • step 2 includes:
  • the first mixed gas into the reaction chamber, and apply DC power less than the first preset value to the target, so that the first mixed gas is ignited to generate plasma, and a bias of the first preset range is applied to the susceptor RF power, and maintain the first set time length, to perform etching pretreatment on the surface of the substrate;
  • etching pretreatment After performing etching pretreatment on the surface of the substrate, increase the DC power applied to the target to make the plasma bombard the target, so as to form a metal nitride film (such as a MoN film) on the etching pretreated substrate.
  • a metal nitride film such as a MoN film
  • the range of the first preset value of the DC power is less than 800W, such as 500W, and the DC power is used to ignite and ionize the first mixed gas to generate plasma.
  • the energetic particles can be used to bombard the substance on the surface of the substrate, so as to perform etching pretreatment on the surface of the substrate.
  • the etching pretreatment can eliminate impurities on the surface of the substrate, and at the same time enhance the mobility of the atomic surface, thereby improving the flatness of the substrate surface, increasing the binding force of the film base, reducing contact resistance and stress, and avoiding film stripping.
  • the above-mentioned first preset range is greater than or equal to 500W and less than or equal to 2500W; the first set duration is, for example, 3s.
  • the application of the bias RF power to the susceptor is stopped, and the DC power applied to the target is increased, for example, to 3000W.
  • the direct current power will form a negative voltage on the target, and promote the ionized first mixed gas to bombard the target, so as to deposit the MoN thin film on the substrate pretreated by etching.
  • the flow range of argon is less than or equal to 100 sccm, preferably less than or equal to 10 sccm; the flow range of krypton is less than or equal to 50 sccm, preferably greater than or equal to 5 sccm, and less than or equal to 30 sccm.
  • the flow rates of argon and krypton can be adjusted respectively by adjusting the gas flow meters corresponding to their respective gas paths, so as to achieve a reasonable setting of the ratio of argon and krypton.
  • argon and krypton The ratio of krypton gas flow is less than or equal to 0.45.
  • the argon gas and krypton gas are fully mixed in the gas mixing chamber and then passed into the reaction chamber, and the process pressure of the reaction chamber is maintained within the range of greater than or equal to 10mTorr and less than or equal to 25mTorr.
  • the above step 3 includes:
  • the above-mentioned second preset value may be 800W, and the DC power may be, for example, 500W.
  • the above-mentioned third preset value may be 1200W, and the radio frequency power may be, for example, 850W; the above-mentioned second set duration is, for example, 5 seconds.
  • the second preset range is greater than or equal to 100W and less than or equal to 500W, such as 240W.
  • the DC power applied to the target is increased to, for example, 1000W.
  • the surface of the deposited Mo film can be bombarded to a certain extent, and the density of the Mo film can be enhanced. , to promote the deposition of high-quality, low-resistivity Mo films, wherein the rate of etching Mo films is less than that of depositing Mo films.
  • the thickness of the Mo thin film is greater than or equal to 150 angstroms and less than or equal to 350 angstroms. By controlling the film thickness within this range, it is easier to obtain a denser and purer low-resistivity Mo film.
  • FIG. 2 is a comparison diagram of the Mo film resistivity obtained in this embodiment and the Mo film resistivity obtained in the prior art, wherein, Thickness is the thickness of the Mo film, and the unit is Angstrom. Resistivity is the resistivity of Mo thin film, the unit is u ⁇ cm. Under the condition that the thickness (Thickness) of the Mo film is 300 angstroms, the resistivity of the Mo film obtained by the prior art is 13.2u ⁇ cm; Compared with the prior art, the resistivity of the Mo film is reduced by 15%-25%.
  • the application range of the Mo film obtained by the method for preparing the metal film provided in this embodiment in the DRAM bit line is expected to be extended to the 1xnm technology node.
  • the metal film obtained by the method for preparing the metal film provided in this embodiment meets the low resistivity requirements of the bit line and the gate layer for the metal film, and the stability of the film performance can further improve the device yield. , to provide more options to solve the bottleneck of the existing technology.
  • FIG. 3 is a schematic diagram of the sheet resistance and its uniformity of the low-resistivity Mo thin film of this embodiment, and the diagram shows the measurement distribution results of 49 points of the sheet resistance of a 12-inch substrate.
  • Fig. 4 is the crystalline XRD pattern of the Mo thin film obtained by the method for preparing the metal thin film provided in this example, and the crystal direction peak of the XRD appears near 2 ⁇ 40.6° and 73.5°, which belong to the body-centered cubic metal Mo[ The diffraction peaks of 110] and [211] crystal directions indicate that the prepared Mo thin film presents a polycrystalline phase structure and [110] preferred orientation growth at the same time. There are no other peaks of other phases, which indicates that a high-purity Mo thin film has been prepared.
  • the method for preparing metal thin films provided by the present invention is not only applicable to the preparation process of molybdenum (Mo) thin films, but also applicable to other advanced metal thin films obtained by PVD magnetron sputtering technology, such as metal ruthenium (Ru) and the like. Alternative materials in the field of memory.

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Abstract

本发明公开了一种物理气相沉积制备金属薄膜的方法，包括：步骤1：将待沉积薄膜的基底放入反应腔室的基座上；步骤2：向反应腔室内通入包括氮气和氪气的第一混合气体，对靶材施加直流功率，使第一混合气体形成等离子体并轰击靶材，以在基底上形成金属氮化物薄膜；步骤3：停止向反应腔室内通入第一混合气体，向反应腔室内通入包括氩气和氪气的第二混合气体，对靶材施加直流功率，使第二混合气体形成等离子体，以在金属氮化物薄膜上形成金属薄膜；对基座施加偏置射频功率，以对金属薄膜的表面进行轰击，提高金属薄膜的致密度。

Description

制备金属薄膜的物理气相沉积方法 技术领域
本发明涉及半导体技术领域，更具体地，涉及一种制备金属薄膜的物理气相沉积方法。
背景技术
近年来，随着动态随机存取存储器(Dynamic Random Access Memory,DRAM)及其关键部件尺寸的不断缩小，部件之间的金属互连及接触等关键尺寸也随之缩减，只有更低电阻率的器件尺寸，才能获得更紧凑、更快速响应的器件结构。DRAM单元按照列(位线，Bit lines)和行(字线，Word lines)的阵列进行运作。位线在感应放大器之间传输电荷，从而编辑(写入)或获得(读取)特定单元的数据。数据写入或从DRAM单元读取数据的速度取决于位线的电阻；电阻越小，数据传输速度越快。导体的电阻取决于电子沿线路运动时遇到的散射点。薄膜中的杂质、颗粒边界和器件表面粗糙度会导致电子运动速度减慢，这些因素对运动速度影响的程度则与薄膜的厚度相关。
在集成电路制造中，常用RC迟滞(resistance-capacitance delay)表示较高阻值带来的影响，器件密度不断增大，金属化互连所带来的RC迟滞会通过各种方式影响器件性能，已经成为阻碍超高密度集成电路效能及速度的关键因素。RC迟滞将降低DRAM结构中位线读取或写入数据的速度，因此，减少RC互连延迟成为近年来半导体行业的主攻方向；随着半导体技术的进步，器件关键尺寸持续不断趋于小型化，尤其在1xnm技术节点的DRAM内存制造中，要求制备更纯净、更光滑、应力可控且高密度的金属薄膜，从而有效解决DRAM尺寸缩小所面临的位线电阻的挑战。
业界通常采用物理气相沉积(Physical Vapor Deposition，PVD)方法制备诸如钨(W)等的金属薄膜，但现有的PVD方法在制备金属薄膜时，存在获得的金属薄膜疏松不致密、电阻率偏高，而且薄膜应力大、膜基结合力差，导致薄膜容易剥落，从而无法满足先进制程的工艺要求。
发明内容
本发明的目的是提出一种制备金属薄膜的物理气相沉积方法，能够增加膜基结合力，防止金属膜剥落，并且薄膜致密度高、结晶好，电阻率低。
为了实现上述目的，本发明提供了一种制备金属薄膜的物理气相沉积方法，包括：
步骤1：将待沉积薄膜的基底放入反应腔室的基座上；
步骤2：向所述反应腔室内通入包括氮气和氪气的第一混合气体，对靶材施加直流功率，使所述第一混合气体形成等离子体并轰击所述靶材，以在所述基底上形成金属氮化物薄膜；
步骤3：停止向所述反应腔室内通入所述第一混合气体，向所述反应腔室内通入包括氩气和氪气的第二混合气体，对所述靶材施加直流功率，以及对所述基座施加偏置射频功率，施加所述直流功率能够使所述第二混合气体形成等离子体并轰击所述靶材，以在所述金属氮化物薄膜上形成金属薄膜；施加所述射频功率能够使所述等离子体对所述金属薄膜的表面进行轰击，以提高所述金属薄膜的致密度。
可选方案中，所述步骤2还包括：对所述基座施加第一预设范围的偏置射频功率，并维持第一设定时长，以对所述基底表面进行刻蚀预处理。
可选方案中，所述步骤2包括：
向所述反应腔室内通入所述第一混合气体，并对所述靶材施加小于第一预设值的直流功率，使所述第一混合气体启辉产生等离子体，以及对所述基座施加所述第一预设范围的偏置射频功率，并维持所述第一设定时长，以对 所述基底表面进行刻蚀预处理；
对所述基底表面进行刻蚀预处理后，增加对所述靶材施加的直流功率，使所述等离子体轰击所述靶材，以在刻蚀预处理后的所述基底上形成所述金属氮化物薄膜。
可选方案中，所述步骤3包括：
对所述靶材施加小于第二预设值的直流功率，使所述第二混合气体启辉形成等离子体；
对所述基座施加小于第三预设值的射频功率，并维持第二设定时长，以对所述金属氮化物薄膜进行刻蚀处理；在所述第二设定时长后，增加对靶材施加的直流功率，使所述等离子体轰击所述靶材，以在所述金属氮化物薄膜上形成所述金属薄膜，同时对所述基座施加第二预设范围的偏置射频功率，以在形成所述金属薄膜的同时刻蚀所述金属薄膜，提高所述金属薄膜的致密度。
可选方案中，在所述步骤3中，所述氩气的流量小于等于100sccm，所述氪气的流量小于等于50sccm。
可选方案中，在所述步骤3中，所述氩气与所述氪气流量的比值小于等于0.45。
可选方案中，在所述步骤2中，所述氪气与所述氮气流量的比值大于等于0.15。
可选方案中，在所述步骤2中，所述氪气的流量小于等于50sccm，所述氩气的流量小于等于200sccm。
可选方案中，在所述步骤2和/或所述步骤3中，对所述靶材施加的直流功率小于等于20000W。
可选方案中，所述步骤1中的工艺条件为：所述反应腔室的真空度小于5×10 -6Torr；所述基座的温度大于等于250℃，且小于等于350℃。
本发明具有以下有益效果：
本发明实施例提供的制备金属薄膜的物理气相沉积方法，通过步骤2先在基底表面形成金属氮化物薄膜，该金属氮化物薄膜不仅可以增加后续沉积的金属薄膜与基底的膜基结合力，避免直接在基底上沉积金属薄膜引起晶格失配，造成金属薄膜剥落，而且还可以使得后续形成的金属薄膜沿[110]晶向择优生长，在器件后段高温热处理工艺时，可以抑制金属薄膜与基底的互扩散现象，从而可以起到阻挡层作用，保证金属薄膜低电阻特性，维持器件性能稳定性并保证良率。同时，上述步骤2采用氮气和氪气(Kr)的第一混合气体形成等离子体，相对于现有技术中的Ar气体，Kr离子的质量较大，由于质量越大，动能越大，这使得靶材被Kr离子轰击后溅射出并沉积在基底上的原子能量越大，从而可以改变低能原子在基底表面的无序状态排布，提高原子在薄膜表面的迁移运动和扩散能力，进而可以提高薄膜致密度、结晶质量，而且提高原子能量还可以使晶粒不断长大，降低电子穿越晶界受到的势垒作用，从而可以显著降低薄膜的电阻率，提高导电性。此外，通过将氮气和氪气混合，不仅可以通过调节二者的比例来降低薄膜电阻率，提高工艺稳定性和灵活性，而且还可以降低使用成本。另外，步骤3中通过对基座施加偏置射频功率，能够使等离子体对金属薄膜的表面进行轰击，以提高金属薄膜的致密度，促进高质量、低电阻率的金属薄膜的沉积。
本发明具有其它的特性和优点，这些特性和优点从并入本文中的附图和随后的具体实施方式中将是显而易见的，或者将在并入本文中的附图和随后的具体实施方式中进行详细陈述，这些附图和具体实施方式共同用于解释本发明的特定原理。
附图说明
通过结合附图对本发明示例性实施例进行更详细的描述，本发明的上述以及其它目的、特征和优势将变得更加明显。
图1示出了根据本发明一实施例的物理气相沉积制备金属薄膜的方法的流程图。
图2示出了现有技术的方法与本发明一实施例的方法形成的金属薄膜电阻率的对比。
图3示出了根据本发明一实施例的金属薄膜的方阻及其均匀性分布图。
图4示出了根据本发明一实施例的金属薄膜的结晶XRD图谱。
具体实施方式
下面将更详细地描述本发明。虽然本发明提供了优选的实施例，然而应该理解，可以以各种形式实现本发明而不应被这里阐述的实施例所限制。相反，提供这些实施例是为了使本发明更加透彻和完整，并且能够将本发明的范围完整地传达给本领域的技术人员。
在本发明的描述中，需要说明的是，术语“中心”、“上”、“下”、“左”、“右”、“竖直”、“水平”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。
在本发明的描述中，需要说明的是，除非另有明确的规定和限定，术语“安装”、“相连”、“连接”应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或一体地连接；可以是机械连接，可以是直接相连，也可以通过中间媒介间接相连。对于本领域的普通技术人员而言，可以具体情况理解上述术语在本发明中的具体含义。
图1示出了本发明一实施例一种制备金属薄膜的物理气相沉积方法的流程图，请参照图1，该方法包括以下步骤：
步骤1：将待沉积薄膜的基底放入反应腔室的基座上；
步骤2：向反应腔室内通入包括氮气和氪气的第一混合气体，对靶材施 加直流功率，使第一混合气体形成等离子体并轰击靶材，以在基底上形成金属氮化物薄膜；
步骤3：停止向反应腔室内通入第一混合气体，向反应腔室内通入包括氩气和氪气的第二混合气体，对靶材施加直流功率，以及对基座施加偏置射频功率，施加上述直流功率能够使第二混合气体形成等离子体并轰击靶材，以在金属氮化物薄膜上形成金属薄膜；施加上述射频功率能够使等离子体对金属薄膜的表面进行轰击，以提高金属薄膜的致密度。
具体地，为了便于理解本方案，首先对用于制备薄膜的设备进行简单的介绍。薄膜的制备在半导体设备的反应腔室中进行，反应腔室中设有基座，用于承载待沉积薄膜的基底，基座中可以具备加热或冷却功能。反应腔室连接有真空系统，真空系统可对反应腔室进行抽气，使反应腔室达到较高的真空度，以满足工艺所需的真空条件。工艺所需的气体通过流量计连接到反应腔室，工艺所需要的靶材被密封在反应腔室的上方区域。沉积金属薄膜的靶材材料可以是纯金属，也可以是金属化合物。进行薄膜沉积时，激励电源会施加激励功率(例如直流功率、射频功率或者二者结合)至靶材，使其相对于接地的反应腔室为负偏压，结合腔室内的高压使气体电离放电而产生带正电的等离子体，带正电的等离子体被靶材吸引并轰击靶材。当等离子体的能量足够高时，会使靶材表面的原子逸出并沉积在基底上，以实现对基底表面的薄膜沉积。
本实施例以在基底表面沉积钼(Mo)薄膜为例，对本发明实施例提供的制备金属薄膜的物理气相沉积方法进行详细说明。
具体地，执行步骤1，根据沉积的薄膜不同，对反应腔室设定适合的工艺条件，将待沉积薄膜的基底放入反应腔室的基座上，将基座温度调至工艺所需的温度。在本实施例中，可选的，基底为氧化硅，用于沉积钼薄膜，设定的工艺条件为，反应腔室的真空度小于5×10 -6Torr；基座的温度大于等于 250℃，且小于等于350℃，优选的，基座的温度为300℃。
可选的，为了能够形成电阻率更低的钼薄膜，可以使用纯度≥99.999wt％的金属Mo靶材，该金属Mo靶材的杂质氧(O)含量≤100wtppm。
执行步骤2，向反应腔室内通入包括氮气和氪气的第一混合气体，对靶材(Mo)施加直流功率，使第一混合气体形成等离子体并轰击靶材，以在基底上形成氮化钼薄膜。
在现有技术中，溅射气体为氩气(Ar)，对靶材施加直流功率后在靶材上形成负电压，促进离化的Ar离子轰击靶材，Mo原子在等离子体区经与Ar离子碰撞、散射，部分散逸到达了基底表面，在基底表面沉积形成Mo薄膜。但是，由Ar离子轰击靶材溅射出并沉积在基底上的Mo原子能量低，且呈无序状态排布，导致薄膜疏松不够致密，电子穿越晶界时受到的势垒作用较强，从而导致Mo薄膜电阻率偏高，无法满足先进制程的工艺要求。同时，现有技术是直接在基底上溅射Mo薄膜，这样会导致Mo薄膜应力大且膜基结合力差，容易剥落。
为了解决上述问题，本实施例中，在形成Mo薄膜之前，先在基底的表面形成氮化钼薄膜，该氮化钼薄膜不仅可以增加后续沉积的Mo薄膜与基底的膜基结合力，避免直接在基底上沉积Mo薄膜引起晶格失配，造成Mo薄膜剥落，而且还可以使得后续形成的Mo薄膜沿[110]晶向择优生长，在器件后段高温热处理工艺时，可以抑制Mo薄膜与基底的互扩散现象，从而可以起到阻挡层作用，保证Mo薄膜低电阻特性，维持器件性能稳定性并保证良率。
同时，上述氮化钼薄膜的制备采用氮气和氪气(Kr)的第一混合气体形成等离子体，相对于现有技术中的Ar气体，Kr离子的质量较大，由于质量越大，动能越大，这使得靶材被Kr离子轰击后溅射出并沉积在基底上的Mo原子能量越大，从而可以改变低能Mo原子在基底表面的无序状态排布，提 高Mo原子在薄膜表面的迁移运动和扩散能力，进而可以提高薄膜致密度、结晶质量，而且提高Mo原子能量还可以使晶粒不断长大，降低电子穿越晶界受到的势垒作用，从而可以显著降低薄膜的电阻率，提高导电性。
此外，通过将氮气和氪气混合，不仅可以通过调节二者的比例(可依据电阻率需求灵活配比)来降低薄膜电阻率，提高工艺稳定性和灵活性，而且还可以节省氪气使用量，降低使用成本。
执行步骤3，停止向反应腔室内通入第一混合气体，向反应腔室内通入包括氩气和氪气的第二混合气体，对靶材施加直流功率，以及对基座施加偏置射频功率，施加直流功率能够使第二混合气体形成等离子体并轰击靶材，以在氮化钼薄膜上形成Mo薄膜；施加射频功率能够使等离子体对Mo薄膜的表面进行轰击，以提高Mo薄膜的致密度。
与步骤2相类似的，上述Mo薄膜的制备采用氩气和氪气(Kr)的第二混合气体形成等离子体，同样可以提高薄膜致密度、结晶质量，并可以显著降低薄膜的电阻率，提高导电性。在步骤2中，通过对基座施加偏置射频功率，可以对形成的氮化钼薄膜以及形成的Mo薄膜表面进行一定的轰击刻蚀(刻蚀速度小于沉积速度)，该刻蚀作用能够在减少薄膜表面缺陷的同时降低薄膜表面粗糙度，以提高金属薄膜的致密度，促进高质量、高致密性的低电阻率Mo薄膜沉积。此外，通过将氩气和氪气混合，不仅可以通过调节二者的比例(可依据电阻率需求灵活配比)来降低薄膜电阻率，提高工艺稳定性和灵活性，而且还可以节省氪气使用量，降低使用成本。
在本实施例中，在步骤2中，可选的，反应腔室的工艺压力维持在大于等于10mTorr，且小于等于25mTorr的范围内，氪气(Kr)的流量范围为小于等于50sccm，优选为小于等于10sccm；氮气的流量范围小于等于200sccm,优选为大于等于10sccm，且小于等于80sccm。
可选方案中，由于氮气比例过低易形成亚稳态MoN薄膜，较难维持工 艺稳定性，通过使氪气与氮气的比例大于等于0.15，可以避免该问题。
本实施例中，生成的氮化钼薄膜的厚度大于等于20埃，且小于等于60埃。通过将氮化钼薄膜的厚度控制在上述范围内，可以减少基底表面缺陷和粗糙度，而且可以在沉积过程中使表面能起主要作用，促进Mo膜柱状大晶粒的成核及长大，有利于Mo薄膜更好的沿[110]晶向方向择优生长。
本实施例中，步骤2包括：
向反应腔室内通入第一混合气体，并对靶材施加小于第一预设值的直流功率，使第一混合气体启辉产生等离子体，以及对基座施加第一预设范围的偏置射频功率，并维持第一设定时长，以对基底表面进行刻蚀预处理；
对基底表面进行刻蚀预处理后，增加对靶材施加的直流功率，使等离子体轰击靶材，以在刻蚀预处理后的基底上形成金属氮化物薄膜(例如MoN薄膜)。
可选的，直流功率的上述第一预设值的范围为小于800W，例如为500W，该直流功率用于使第一混合气体启辉电离，产生等离子体。
上述步骤2中，通过对基座施加第一预设范围的偏置射频功率，可以通过荷能粒子对基底表面物质进行轰击，以对基底表面进行刻蚀预处理。该刻蚀预处理可以消除基底表面上的杂质，同时增强原子表面迁移率，从而可以提高基底表面的平整度，增加膜基结合力，减少接触电阻及应力，避免脱膜现象。可选的，上述第一预设范围为大于等于500W，且小于等于2500W；第一设定时长例如为3s。
对基底表面进行上述预处理后(即，经过第一设定时长)，停止对基座施加偏置射频功率，并增加对靶材施加的直流功率，例如增加至3000W。该直流功率会在靶材上形成负电压，促进离化的第一混合气体轰击靶材，以在经刻蚀预处理后的基底上进行MoN薄膜的沉积。
在一个实施例中，在上述步骤3中，氩气的流量范围为小于等于 100sccm，优选为小于等于10sccm；氪气的流量范围为小于等于50sccm,优选为大于等于5sccm，且小于等于30sccm。在实际应用中，可以通过调节氩气和氪气各自气路对应的气体流量计，来分别调节二者的流量，以实现氩气和氪气配比的合理设置，本实施例中氩气与氪气流量的比值小于等于0.45。氩气与氪气经混气室充分混匀后通入反应腔室，且将反应腔室的工艺压力维持在大于等于10mTorr，且小于等于25mTorr范围内。
在一个实施例中，上述步骤3包括：
对靶材施加小于第二预设值的直流功率，使第二混合气体启辉形成等离子体；
对基座施加小于第三预设值的射频功率，并维持第二设定时长，以对MoN薄膜进行刻蚀处理；在第二设定时长后，增加对靶材施加的直流功率，使等离子体轰击所述靶材，以在金属氮化物薄膜上形成Mo薄膜，同时对基座施加第二预设范围的偏置射频功率，以在形成Mo薄膜的同时刻蚀Mo薄膜，提高Mo薄膜的致密度。
可选的，上述步骤3中，上述第二预设值可以为800W，直流功率例如为500W。
可选的，上述第三预设值可以为1200W，射频功率例如为850W；上述第二设定时长例如为5秒。
通过对MoN薄膜进行刻蚀处理，有利于降低MoN薄膜与Mo薄膜的欧姆接触，降低界面能并形成较小的附加阻抗，从而有利于低电阻率Mo薄膜的形成。
可选的，上述步骤3中，上述第二预设范围为大于等于100W，且小于等于500W，例如240W。
可选的，上述步骤3中，增加对靶材施加的直流功率例如增加至1000W。
在第二设定时长后，通过增加对靶材施加的直流功率，同时对基座施加 第二预设范围的偏置射频功率，可以对沉积的Mo薄膜表面进行一定轰击，增强Mo薄膜致密度，促进高质量、低电阻率的Mo薄膜沉积，其中，刻蚀Mo薄膜的速度小于沉积Mo薄膜的速度。
可选的，Mo薄膜的厚度大于等于150埃，且小于等于350埃。通过将薄膜厚度控制在该范围内，更容易获得更致密、更纯净的低电阻率Mo薄膜。
参考图2，图2为本实施例获得的Mo薄膜电阻率与现有技术获得的Mo薄膜电阻率的对比图，其中，Thickness为Mo薄膜的厚度，单位为埃。Resistivity为Mo薄膜的电阻率，单位为uΩ·cm。在Mo薄膜的厚度(Thickness)为300埃的条件下，现有技术获得的Mo薄膜电阻率为13.2uΩ·cm；本实施例获得的Mo薄膜电阻率为10.1uΩ·cm，本实施例获得的Mo薄膜电阻率与现有技术相比，下降15％-25％，通过本实施例提供的制备金属薄膜的方法获得的Mo薄膜在DRAM位线中的应用范围有望扩展至1xnm技术节点。在17nm节点及以下的DRAM领域，本实施例提供的制备金属薄膜的方法获得的金属薄膜满足位线及栅极层对金属薄膜的低电阻率要求，薄膜性能的稳定性可进一步提高器件良率，为解决现有技术的瓶颈提供更多选择。
参考图3，图3为本实施例低电阻率Mo薄膜的方阻及其均匀性示意图，图示为12寸基底的方块电阻49点量测分布结果。图示方块电阻值Rs＝3.35Ω/sq，方阻均匀性(1sigma；％)＝1.869％，可见，通过本实施例提供的制备金属薄膜的方法获得的Mo薄膜，可以达到半导体制造工艺对位线及栅极工艺均匀性的要求。
参考图4，图4为通过本实施例提供的制备金属薄膜的方法获得的Mo薄膜的结晶XRD图谱，XRD晶向峰位在2θ≈40.6°、73.5°附近出现了属于体心立方金属Mo[110]、[211]晶向的衍射峰，说明制备得到的Mo薄膜呈现多晶相结构，同时呈现[110]择优取向生长，除氧化硅基底在≈70°左右出现大的 非晶包外，无其它物相的杂峰，这表明制备得到了高纯度的Mo薄膜。
本发明提供的制备金属薄膜的方法不仅适用于钼(Mo)薄膜的制备工艺，也适用于其它与采用PVD磁控溅射技术获得低电阻率的金属薄膜，如金属钌(Ru)等的先进存储器领域的可替代性材料。
以上已经描述了本发明的各实施例，上述说明是示例性的，并非穷尽性的，并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和精神的情况下，对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的。

Claims (10)

  1. 一种制备金属薄膜的物理气相沉积方法，其特征在于，所述方法包括：
    步骤1：将待沉积薄膜的基底放入反应腔室的基座上；
    步骤2：向所述反应腔室内通入包括氮气和氪气的第一混合气体，对靶材施加直流功率，使所述第一混合气体形成等离子体并轰击所述靶材，以在所述基底上形成金属氮化物薄膜；
    步骤3：停止向所述反应腔室内通入所述第一混合气体，向所述反应腔室内通入包括氩气和氪气的第二混合气体，对所述靶材施加直流功率，以及对所述基座施加偏置射频功率，施加所述直流功率能够使所述第二混合气体形成等离子体并轰击所述靶材，以在所述金属氮化物薄膜上形成金属薄膜；施加所述射频功率能够使所述等离子体对所述金属薄膜的表面进行轰击，以提高所述金属薄膜的致密度。
  2. 根据权利要求1所述的方法，其特征在于，所述步骤2还包括：对所述基座施加第一预设范围的偏置射频功率，并维持第一设定时长，以对所述基底表面进行刻蚀预处理。
  3. 根据权利要求2所述的方法，其特征在于，所述步骤2包括：
    向所述反应腔室内通入所述第一混合气体，并对所述靶材施加小于第一预设值的直流功率，使所述第一混合气体启辉产生等离子体，以及对所述基座施加所述第一预设范围的偏置射频功率，并维持所述第一设定时长，以对所述基底表面进行刻蚀预处理；
    对所述基底表面进行刻蚀预处理后，增加对所述靶材施加的直流功率，使所述等离子体轰击所述靶材，以在刻蚀预处理后的所述基底上形成所述金属氮化物薄膜。
  4. 根据权利要求1所述的方法，其特征在于，所述步骤3包括：
    对所述靶材施加小于第二预设值的直流功率，使所述第二混合气体启辉形成等离子体；
    对所述基座施加小于第三预设值的射频功率，并维持第二设定时长，以对所述金属氮化物薄膜进行刻蚀处理；在所述第二设定时长后，增加对靶材施加的直流功率，使所述等离子体轰击所述靶材，以在所述金属氮化物薄膜上形成所述金属薄膜，同时对所述基座施加第二预设范围的偏置射频功率，以在形成所述金属薄膜的同时刻蚀所述金属薄膜，提高所述金属薄膜的致密度。
  5. 根据权利要求1所述的方法，其特征在于，在所述步骤3中，所述氩气的流量小于等于100sccm，所述氪气的流量小于等于50sccm。
  6. 根据权利要求1所述的方法，其特征在于，在所述步骤3中，所述氩气与所述氪气流量的比值小于等于0.45。
  7. 根据权利要求1所述的方法，其特征在于，在所述步骤2中，所述氪气与所述氮气流量的比值大于等于0.15。
  8. 根据权利要求1所述的方法，其特征在于，在所述步骤2中，所述氪气的流量小于等于50sccm，所述氩气的流量小于等于200sccm。
  9. 根据权利要求1所述的方法，其特征在于，在所述步骤2和/或所述步骤3中，对所述靶材施加的直流功率小于等于20000W。
  10. 根据权利要求1所述的方法，其特征在于，所述步骤1中的工艺条 件为：所述反应腔室的真空度小于5×10 -6Torr；所述基座的温度大于等于250℃，且小于等于350℃。
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