CN114369805A - Magnetron sputtering preparation of high-surface-quality HfO2Method for base mixing thin film - Google Patents

Magnetron sputtering preparation of high-surface-quality HfO2Method for base mixing thin film Download PDF

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CN114369805A
CN114369805A CN202210038951.2A CN202210038951A CN114369805A CN 114369805 A CN114369805 A CN 114369805A CN 202210038951 A CN202210038951 A CN 202210038951A CN 114369805 A CN114369805 A CN 114369805A
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target
sputtering
hfo
film
magnetron sputtering
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CN114369805B (en
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杨勇
吕晓城
黄政仁
刘桂玲
魏玉全
姚秀敏
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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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
    • C23C14/35—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
    • 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
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/10—Nuclear fusion reactors

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

The invention provides a method for preparing high-surface-quality HfO by magnetron sputtering2Method for producing a hybrid thin film, HfO produced by means of dual-target magnetron sputtering2Based on a mixed film. HfO of the invention2The base mixed film has superior surface quality.

Description

Magnetron sputtering preparation of high-surface-quality HfO2Method for base mixing thin film
Technical Field
The invention relates to the field of materials, in particular to a method for preparing high-surface-quality HfO by magnetron sputtering2A method of base mixing a thin film.
Background
In recent years, with the research requirements of various countries on controllable nuclear fusion, simulated explosion, laser weapons and the like, the realization of high-power and high-energy strong laser beams is particularly urgent, and more rigorous requirements are provided for the design and related elements of a laser driving system. The high-energy laser is realized by plating a dielectric multilayer film with high refractive index and low refractive index alternately on a laser resonant cavity and adjusting the phase of light to prepare a high-reflection film meeting the requirement.
HfO2Because of its higher refractive index, low absorption, scattering and high transmittance in the ultraviolet visible and near infrared bands, it is commonly used as a high refractive index material in laser reflective films, but because of the better crystallinity and larger surface roughness of the deposited films, the scattering of the films is increased, and it is difficult to meet the performance requirements of laser reflective films.
At present, the required HfO is mainly prepared by thermal evaporation, ion plating and magnetron sputtering methods2A film. The film prepared by thermal evaporation has loose structure and poor density, and impurity ions are easily introduced in the ion plating. Compared with the former two methods, the magnetron sputtering method has the technical advantages of high controllability, simple process and the like, can prepare mixed films with different components and chemical proportions, and is widely applied to the preparation of the mixed films.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for preparing high-surface-quality HfO by magnetron sputtering with low surface roughness and high surface quality2A method of base mixing a thin film.
According to one aspect of the invention, the invention provides a method for preparing high-surface-quality HfO by magnetron sputtering2A method of base mixing a film comprising the steps of:
step 1, cleaning a monocrystalline silicon substrate;
step 2, using HfO2Target and Nb2O5Pre-sputtering the target material by the target;
step 3, using HfO2Target and Nb2O5Sputtering a monocrystalline silicon substrate by a target to obtain a mixed Hf/Nb film by deposition, wherein the HfO is prepared by2The target sputtering power is 50-250 w, and the Nb is2O5The target sputtering power is 50-250 w.
Preferably: HfO in the step 32The target sputtering power is 200-250 w.
Preferably: nb in the step 32O5The target sputtering power is 100-200 w.
Preferably: the sputtering time in the step 3 is 30-120 min.
Preferably: the sputtering time in the step 3 is 60-90 min.
Preferably: the target base distance in the step 3 is 100 mm-140 mm.
Preferably: the sputtering angle between the target and the substrate in the step 3 is 27-31 degrees.
Preferably: the purity of the HfO2 target and the purity of the Nb2O5 target in the step 3 are both more than 99.5 percent.
Preferably: the step 1 comprises the following steps:
step 1.1, carrying out ultrasonic cleaning on a monocrystalline silicon substrate;
and 1.2, carrying out radio frequency cleaning on the monocrystalline silicon substrate in a vacuum environment.
Preferably: the root mean square roughness of the mixed film formed in the step 3 is 0.1-2.0 nm, and the average roughness is 0.1-1.0 nm.
The invention discloses a method for preparing a high-surface-quality HFO 2-based mixed film by magnetron sputtering, which is based on HfO2The surface quality of the film is poor, and the like, a double-target co-sputtering method is adopted, and HfO is changed2Sputtering power of target material, Nb2O5The sputtering power of the target is used for obtaining the mixed film with low surface roughness and high surface quality.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, with reference to the accompanying drawings.
FIG. 1 shows HfO prepared according to an embodiment of the present invention2Base mixed thin film SEM (secondary electron image) test results;
FIG. 2 shows HfO prepared according to an embodiment of the present invention2The results were measured by a mixed thin film AFM (atomic force microscope).
Detailed Description
Example embodiments will now be described more fully with reference to the accompanying drawings. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art. The same reference numerals in the drawings denote the same or similar structures, and thus their repetitive description will be omitted.
In the embodiment of the invention, the magnetron sputtering method for preparing the high-surface-quality HfO is provided2The method of the base mixed film can be carried out on HfO by a magnetron sputtering method, a double-target co-sputtering method and the change of the sputtering power of a target material2A certain amount of Nb is doped on the basis of a film2O5Compared with HfO2Film, deposited HfO2The surface roughness of the base mixed film is lower, the surface quality is higher, the light wave scattering of the film is reduced, the requirement of the laser reflection film on the surface quality of a high-refractive-index material can be met, and the HfO is widened2The film has application prospect in the field of optical films.
The method comprises the following steps:
step 1.1, carrying out ultrasonic cleaning on a monocrystalline silicon substrate; preferably, the monocrystalline silicon substrate is sequentially placed in deionized water, acetone and alcohol for ultrasonic cleaning, and the surface of the substrate is wiped by dust-free cloth stained with alcohol until the substrate is completely clean;
the ultrasonic cleaning time is preferably 10-30 min, and preferably 20 min.
And 1.2, carrying out radio frequency cleaning on the monocrystalline silicon substrate in a vacuum environment. Preferably, the coating machine is pumped to the background vacuum, the cleaned substrate is placed into a magnetron sputtering furnace, argon is introduced, and radio frequency cleaning is carried out;
preferably, the background vacuum is pumped to 1 x 10 < -3 > Pa to 1 x 10 < -4 > Pa, preferably, the background vacuum is 1 x 10 < -4 > Pa, and the sputtering molecules can be effectively inhibited from reacting with gas in the air to introduce impurities as the vacuum degree is higher.
Preferably, the power of the radio frequency cleaning is 50 w-250 w, preferably 100w, and the time is 2-4 min, and preferably 3 min.
The ultrasonic cleaning and the radio frequency cleaning are used for removing impurities on the surface of the substrate and providing an ultra-clean base for coating. The purpose of the vacuum treatment is to reduce collision and reaction between sputtered molecules and residual gas molecules and provide a vacuum degree meeting the requirement for sputtering reaction. Too short a cleaning time results in impurities remaining on the surface of the substrate, and too long a cleaning time may damage the substrate.
Step 2, using HfO2Target and Nb2O5Pre-sputtering the target material by the target; preferably, high-purity HfO2 and Nb2O5 targets are respectively arranged in a magnetron sputtering furnace, the target base distance and the sputtering angle between the targets and a substrate are fixed, a certain amount of argon is introduced, the working air pressure is kept unchanged, and the targets are pre-sputtered by double targets at a certain power;
the purpose of pre-sputtering is to remove impurities from the target surface.
Preferably, the target base distance is 100 mm-140 mm, the sputtering angle between the target and the substrate is 27-31 degrees, and the HfO2Target and Nb2O5The target purity is more than 99.5 percent, the preferred target base distance is 120mm, the sputtering angle of the target and the substrate is 29 degrees, and the target purity is 99.99 percent. The double-target pre-sputtering power is 50-250 w, preferably 250w, and the pre-sputtering time is 5-30 min, preferably 10 min.
Step 3, using HfO2Target and Nb2O5Sputtering the monocrystalline silicon substrate by the target, and depositing to obtain the Hf/Nb mixed film.
HfO2The target sputtering power is 50 to 250w, preferably 200 to 250w, and preferably 250 w.
Nb2O5The target sputtering power is 50 to 250w, preferably 100 to 200w, and preferably 100 w.
The sputtering time is preferably 30 to 120min, more preferably 60 to 90min, and more preferably 60 min.
The flow of argon gas required by radio frequency cleaning, pre-sputtering and sputtering is 10-30 sccm, the working pressure is 0.4-0.6 Pa, the rotation speed of the sample plate is 5-20 r/min, preferably the flow of argon gas is 20sccm, the working pressure is 0.5Pa, and the rotation speed of the sample plate is 10 r/min.
Too slow or too fast a rotation of the sample plate may result in non-uniform coating of the substrate. Too low a working pressure can lead to the deposition film being loose, and too high a working pressure can lead to the deposition rate of a certain area of the film being too fast, leading to the localized preferential growth of the film and the rough surface of the film.
The root mean square roughness of the finally formed mixed film is 0.1-2.0 nm, and the average roughness is 0.1-1.0 nm.
The embodiment of the invention discloses a method for preparing high-surface-quality HfO by magnetron sputtering2Method for forming a hybrid film by using HfO by magnetron sputtering2、Nb2O5For the target material, cleaning a monocrystalline silicon wafer substrate, pre-sputtering the target material and sputtering, and changing HfO2、Nb2O5Sputtering the target material with power, and depositing for a certain time to obtain the mixed films with different Hf/Nb chemical ratios. Deposited hybrid film phase vs HfO2The film has lower surface roughness and higher surface quality.
The invention is described below in specific examples:
example 1
(1) Cleaning of substrates
And (3) selecting a monocrystalline silicon substrate, sequentially putting deionized water, acetone and alcohol into the monocrystalline silicon substrate, ultrasonically cleaning the monocrystalline silicon substrate for 20min, and wiping the monocrystalline silicon substrate by using dust-free cloth until no obvious stain exists on the surface of the film.
And (3) putting the monocrystalline silicon substrate into a magnetron sputtering furnace, turning on a radio frequency power supply, and introducing argon gas for radio frequency cleaning. The argon flow is 20sccm, the radio frequency cleaning power is 100w, and the radio frequency cleaning time is 3 min.
(2) Pre-sputtering of target material
Respectively adding high-purity HfO2、Nb2O5The target material is put into a magnetron sputtering furnace, the target base distance is fixed to be 120mm, the angle between the target material and the substrate is fixed to be 29 degrees, a baffle plate is closed, a radio frequency power supply is opened, argon is introduced, and the target material is pre-sputtered for a certain time to remove impurities on the surface of the target material. The argon flow is 20sccm, the pre-sputtering power is 250w, and the pre-sputtering time is 10 min.
(3) Sputtering of target materials
Loading the substrate into the sputtering chamberIn the shooting chamber, the air pressure of the chamber is pumped to the background vacuum of 1X 10-4Pa, setting the flow of argon and adjusting the baffle valve to the working pressure of 0.5 Pa. Opening the baffle, turning on the RF power supply, and setting HfO2、Nb2O5Sputtering is carried out by the sputtering power of the target material.
Argon flow 20sccm, HfO2The sputtering power of the target is 250w, Nb2O5The sputtering power of the target is 100w, and the sputtering time is 60 min.
Prepared HfO2The root mean square roughness RMS of the base mixed film was 0.423nm, and the average roughness Ra was 0.331 nm.
FIG. 1 is HfO prepared in example 12SEM images of the base mixed films showed that: the prepared film has smooth surface, compact accumulation and no obvious gap.
FIG. 2 is HfO prepared in example 12Based on the mixed thin film AFM image, the results show that: the prepared film has smaller surface particles, dense distribution and smaller roughness.
Example 2
(1) Cleaning of substrates
And (3) selecting a monocrystalline silicon substrate, sequentially putting deionized water, acetone and alcohol into the monocrystalline silicon substrate, ultrasonically cleaning the monocrystalline silicon substrate for 20min, and wiping the monocrystalline silicon substrate by using dust-free cloth until no obvious stain exists on the surface of the film.
And (3) putting the monocrystalline silicon substrate into a magnetron sputtering furnace, turning on a radio frequency power supply, and introducing argon gas for radio frequency cleaning. The argon flow is 25sccm, the radio frequency cleaning power is 50w, and the radio frequency cleaning time is 4 min.
(2) Pre-sputtering of target material
Respectively adding high-purity HfO2、Nb2O5The target material is put into a magnetron sputtering furnace, the target base distance is fixed to be 120mm, the angle between the target material and the substrate is fixed to be 27 degrees, a baffle plate is closed, a radio frequency power supply is opened, argon is introduced, and the target material is pre-sputtered for a certain time to remove impurities on the surface of the target material. The argon flow is 25sccm, the pre-sputtering power is 200w, and the pre-sputtering time is 15 min.
(3) Sputtering of target materials
Loading the substrate into a sputtering chamber, and pumping the chamber to atmospheric pressureBackground vacuum 3X 10-4Pa, setting the flow of argon and adjusting the baffle valve to the working pressure of 0.4 Pa. Opening the baffle, turning on the RF power supply, and setting HfO2、Nb2O5Sputtering is carried out by the sputtering power of the target material. Argon flow 25sccm, HfO2The sputtering power of the target material is 200w, Nb2O5The sputtering power of the target is 160w, and the sputtering time is 75 min.
Example 3
(1) Cleaning of substrates
And (3) selecting a monocrystalline silicon substrate, sequentially putting deionized water, acetone and alcohol into the monocrystalline silicon substrate, ultrasonically cleaning the monocrystalline silicon substrate for 20min, and wiping the monocrystalline silicon substrate by using dust-free cloth until no obvious stain exists on the surface of the film. And (3) putting the monocrystalline silicon substrate into a magnetron sputtering furnace, turning on a radio frequency power supply, and introducing argon gas for radio frequency cleaning. The argon flow is 15sccm, the radio frequency cleaning power is 250w, and the radio frequency cleaning time is 2 min.
(2) Pre-sputtering of target material
Respectively adding high-purity HfO2、Nb2O5The target material is put into a magnetron sputtering furnace, the target base distance is fixed to be 120mm, the angle between the target material and the substrate is fixed to be 31 degrees, a baffle plate is closed, a radio frequency power supply is opened, argon is introduced, and the target material is pre-sputtered for a certain time to remove impurities on the surface of the target material. The argon flow is 15sccm, the pre-sputtering power is 150w, and the pre-sputtering time is 20 min.
(3) Sputtering of target materials
Loading the substrate into a sputtering chamber, evacuating the chamber to a background vacuum of 5X 10-4Pa, setting the flow of argon and adjusting the baffle valve to the working pressure of 0.6 Pa. Opening the baffle, turning on the RF power supply, and setting HfO2、Nb2O5Sputtering is carried out by the sputtering power of the target material. Argon flow 15sccm, HfO2The sputtering power of the target material is 150w, Nb2O5The sputtering power of the target is 150w, and the sputtering time is 90 min.
Example 4
(1) Cleaning of substrates
And (3) selecting a monocrystalline silicon substrate, sequentially putting deionized water, acetone and alcohol into the monocrystalline silicon substrate, ultrasonically cleaning the monocrystalline silicon substrate for 20min, and wiping the monocrystalline silicon substrate by using dust-free cloth until no obvious stain exists on the surface of the film. And (3) putting the monocrystalline silicon substrate into a magnetron sputtering furnace, turning on a radio frequency power supply, and introducing argon gas for radio frequency cleaning. The argon flow is 10sccm, the radio frequency cleaning power is 250w, and the radio frequency cleaning time is 3 min.
(2) Pre-sputtering of target material
Respectively adding high-purity HfO2、Nb2O5The target material is put into a magnetron sputtering furnace, the target base distance is fixed to be 120mm, the angle between the target material and the substrate is fixed to be 28 degrees, a baffle plate is closed, a radio frequency power supply is opened, argon is introduced, and the target material is pre-sputtered for a certain time to remove impurities on the surface of the target material. The argon flow is 10sccm, the pre-sputtering power is 200w, and the pre-sputtering time is 20 min.
(3) Sputtering of target materials
Loading the substrate into a sputtering chamber, evacuating the chamber to a background vacuum of 2X 10-4Pa, setting the flow of argon and adjusting the baffle valve to the working pressure of 0.5 Pa. Opening the baffle, turning on the RF power supply, and setting HfO2、Nb2O5Sputtering is carried out by the sputtering power of the target material. Argon flow 15sccm, HfO2The sputtering power of the target material is 150w, Nb2O5The sputtering power of the target is 120w, and the sputtering time is 120 min.
Example 5
(1) Cleaning of substrates
And (3) selecting a monocrystalline silicon substrate, sequentially putting deionized water, acetone and alcohol into the monocrystalline silicon substrate, ultrasonically cleaning the monocrystalline silicon substrate for 20min, and wiping the monocrystalline silicon substrate by using dust-free cloth until no obvious stain exists on the surface of the film. And (3) putting the monocrystalline silicon substrate into a magnetron sputtering furnace, turning on a radio frequency power supply, and introducing argon gas for radio frequency cleaning. The argon flow is 20sccm, the radio frequency cleaning power is 200w, and the radio frequency cleaning time is 2 min.
(2) Pre-sputtering of target material
Respectively adding high-purity HfO2、Nb2O5The target material is put into a magnetron sputtering furnace, the target base distance is fixed to be 120mm, the angle between the target material and the substrate is fixed to be 30 degrees, a baffle plate is closed, a radio frequency power supply is turned on, argon is introduced, and the target material is pre-sputtered for a certain time to remove impurities on the surface of the target material. Argon flow is 15sccm, the pre-sputtering power is 200w,the pre-sputtering time is 20 min.
(3) Sputtering of target materials
Loading the substrate into a sputtering chamber, evacuating the chamber to a background vacuum of 4X 10-4Pa, setting the flow of argon and adjusting the baffle valve to the working pressure of 0.4 Pa. Opening the baffle, turning on the RF power supply, and setting HfO2、Nb2O5Sputtering is carried out by the sputtering power of the target material. Argon flow 20sccm, HfO2The sputtering power of the target is 160w, Nb2O5The sputtering power of the target is 180w, and the sputtering time is 90 min.
Comparative example 1
Comparative example 1 is prepared identically to example 1, except that: HfO2The sputtering power of the target is 250w, Nb2O5The sputtering power of the target is 0w, the root mean square roughness RMS of the prepared film is 5.836nm, and the average roughness Ra is 4.725 nm.
Comparative example 2
Comparative example 2 is prepared identically to example 1, except that: HfO2The sputtering power of the target material is 25w, Nb2O5The sputtering power of the target is 250w, the root mean square roughness RMS of the prepared film is 3.745nm, and the average roughness Ra is 2.896 nm.
Table 1 below shows the RMS and Ra test results for the films prepared in examples 1-5 and comparative examples 1-2, showing that: HfO prepared according to examples 1-5 of the invention2The root mean square roughness RMS and the average roughness Ra of the base mixed film were low.
Table 1: RMS and Ra test results Table
Sample numbering RMS(nm) Ra(nm)
Example 1 0.423 0.331
Example 2 0.680 0.543
Example 3 0.874 0.695
Example 4 0.636 0.503
Example 5 0.712 0.560
Comparative example 1 5.836 4.725
Comparative example 2 3.745 2.896
In summary, the method for preparing the HFO 2-based mixed thin film with high surface quality by magnetron sputtering according to the embodiment of the present invention is that the HFO 2-based mixed thin film prepared by magnetron sputtering has superior surface quality.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims (10)

1. Magnetron sputtering preparation of high-surface-quality HfO2A method of base mixing a film, comprising the steps of:
step 1, cleaning a monocrystalline silicon substrate;
step 2, using HfO2Target and Nb2O5Pre-sputtering the target material by the target;
step 3, using HfO2Target and Nb2O5Sputtering a monocrystalline silicon substrate by a target to obtain a mixed Hf/Nb film by deposition, wherein the HfO is prepared by2The target sputtering power is 50-250 w, and the Nb is2O5The target sputtering power is 50-250 w.
2. The magnetron sputtering process for preparing high surface quality HfO according to claim 12A method of base mixing a film, characterized by: HfO in the step 32The target sputtering power is 200-250 w.
3. The magnetron sputtering process for preparing high surface quality HfO according to claim 12A method of base mixing a film, characterized by: nb in the step 32O5The target sputtering power is 100-200 w.
4. The magnetron sputtering process for preparing high surface quality HfO according to claim 12A method of base mixing a film, characterized by: the sputtering time in the step 3 is 30-120 min.
5. The magnetron sputtering process for preparing HfO with high surface quality according to claim 42A method of base mixing a film, characterized by: the sputtering time in the step 3 is 60-90 min.
6. The magnet of claim 1Controlled sputtering preparation of high surface quality HfO2A method of base mixing a film, characterized by: the target base distance in the step 3 is 100 mm-140 mm.
7. The magnetron sputtering process for preparing high surface quality HfO according to claim 12A method of base mixing a film, characterized by: the sputtering angle between the target and the substrate in the step 3 is 27-31 degrees.
8. The magnetron sputtering process for preparing high surface quality HfO according to claim 12A method of base mixing a film, characterized by: the purity of the HfO2 target and the purity of the Nb2O5 target in the step 3 are both more than 99.5 percent.
9. The magnetron sputtering process for preparing high surface quality HfO according to claim 12A method of base mixing a film, characterized by: the step 1 comprises the following steps:
step 1.1, carrying out ultrasonic cleaning on a monocrystalline silicon substrate;
and 1.2, carrying out radio frequency cleaning on the monocrystalline silicon substrate in a vacuum environment.
10. The magnetron sputtering process for preparing high surface quality HfO according to claim 12A method of base mixing a film, characterized by: the root mean square roughness of the mixed film formed in the step 3 is 0.1-2.0 nm, and the average roughness is 0.1-1.0 nm.
CN202210038951.2A 2022-01-13 2022-01-13 Magnetron sputtering preparation of high-surface-quality HfO 2 Method for base mixing thin film Active CN114369805B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100279124A1 (en) * 2008-10-31 2010-11-04 Leybold Optics Gmbh Hafnium or zirconium oxide Coating
CN108441830A (en) * 2018-03-01 2018-08-24 大连理工大学 A method of hafnium oxide based ferroelectric film is prepared using reaction magnetocontrol sputtering
CN109638154A (en) * 2018-12-17 2019-04-16 湖北大学 A kind of flexible gating tube device and preparation method thereof based on hafnium titanyl laminated film
CN113025959A (en) * 2021-03-07 2021-06-25 中国航空制造技术研究院 Method for preparing hafnium oxide-based ferroelectric film at low temperature by ion beam assisted magnetron sputtering deposition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100279124A1 (en) * 2008-10-31 2010-11-04 Leybold Optics Gmbh Hafnium or zirconium oxide Coating
CN108441830A (en) * 2018-03-01 2018-08-24 大连理工大学 A method of hafnium oxide based ferroelectric film is prepared using reaction magnetocontrol sputtering
CN109638154A (en) * 2018-12-17 2019-04-16 湖北大学 A kind of flexible gating tube device and preparation method thereof based on hafnium titanyl laminated film
CN113025959A (en) * 2021-03-07 2021-06-25 中国航空制造技术研究院 Method for preparing hafnium oxide-based ferroelectric film at low temperature by ion beam assisted magnetron sputtering deposition

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LUN XU ET AL.: "Kinetic pathway of the ferroelectric phase formation in doped HfO2 films", 《JOURNAL OF APPLIED PHYSICS》 *
李智等: "射频磁控溅射制备HfLaO薄膜结构和光学性能研究", 《无机材料学报》 *

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