CN114438458A - Preparation method of hafnium oxide film - Google Patents
Preparation method of hafnium oxide film Download PDFInfo
- Publication number
- CN114438458A CN114438458A CN202011206543.0A CN202011206543A CN114438458A CN 114438458 A CN114438458 A CN 114438458A CN 202011206543 A CN202011206543 A CN 202011206543A CN 114438458 A CN114438458 A CN 114438458A
- Authority
- CN
- China
- Prior art keywords
- workpiece
- plated
- hafnium oxide
- hafnium
- oxide film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910000449 hafnium oxide Inorganic materials 0.000 title claims abstract description 32
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 7
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 238000007733 ion plating Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 239000010937 tungsten Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 36
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 18
- 229910052735 hafnium Inorganic materials 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 238000010894 electron beam technology Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000005684 electric field Effects 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000001706 oxygenating effect Effects 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000010849 ion bombardment Methods 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 9
- 238000005566 electron beam evaporation Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 238000004544 sputter deposition Methods 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 241000059630 Nodularia <Cyanobacteria> Species 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Images
Classifications
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
-
- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- 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
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a method for preparing a hafnium oxide film by using a three-stage low-pressure reactive ion plating method, which comprises the following steps: preparing a workpiece to be plated, cleaning and activating ions of the workpiece to be plated, and coating, wherein a tripolar low-pressure reaction ion plating device is used, and the device comprises a workpiece table, a clamp, an evaporation crucible, a pulse direct-current power supply, a tungsten filament, a direct-current power supply and an air inlet; the method solves the problem of film material sputtering when the hafnium oxide film is plated by the traditional electron beam evaporation process, reduces the node defect probability which possibly occurs when the hafnium oxide film is deposited, and improves the laser damage threshold of the film.
Description
Technical Field
The invention relates to the field of optical coating, in particular to a preparation method of a hafnium oxide film.
Background
In modern optical systems, the coated optical element is often the weakest ring due to material and process limitations, especially in high power lasers, where the performance of the coated optical element largely determines the stability of the overall laser system. Hafnium oxide (HfO)2) The material has the advantages of high melting point, high thermal stability, wide transmittance range and the like, and is widely selected as a high-refractive-index material of a high-power laser film product. The current mainstream technology adopts the method of electron beam direct Evaporation (E-beam Evaporation) hafnium oxide granular/block film material for plating, and sometimes ion is used as an auxiliary materialAnd (4) beam bombardment. However, when the electron beam evaporation method is used to plate the hafnium oxide thin film, the residual gas in the hafnium oxide film material is released and the volume change caused by the phase change of the hafnium oxide due to different temperatures (about 2200 ℃ at the melting point of the film material at the top of the crucible and about 100 ℃ at the bottom) can cause the splashing of small particles of the film material. Nodule defects (nodularia defects) are generated after the film is wrapped by a subsequent film layer, and the Laser Damage Threshold (LDT) of the film layer is seriously reduced.
Therefore, how to provide a method for preparing a hafnium oxide thin film for obtaining better plating performance and solving the problems of high probability of node defect occurrence, reduced laser damage threshold of a film layer and the like after subsequent film layer wrapping is the technical problem to be solved by the invention.
Disclosure of Invention
Aiming at the defects and problems in the prior art, the invention aims to provide a method for preparing a hafnium oxide film, which aims to obtain better plating performance and solve the problems of high probability of nodule defects after subsequent film coating, reduction of laser damage threshold of the film and the like, and the technical problem to be solved by the invention is solved.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing a hafnium oxide thin film comprises the following steps:
first, preparation of workpiece to be plated
Placing a workpiece to be plated in acetone and isopropanol solutions in sequence, performing ultrasonic cleaning for 10 minutes respectively, and then drying the workpiece by using dry argon to remove oil stains, impurities and the like attached to the surface of the workpiece to be plated;
secondly, ion cleaning and activation of the workpiece to be plated
(1) Placing the processed workpiece to be plated on a rotary base body table in a vacuum chamber for fixing, and vacuumizing the cavity of the vacuum chamber to 2 x 10-3Introducing oxygen after Pa, and maintaining the pressure of the vacuum chamber at 3 Pa;
(2) opening the workpiece table bias device, applying medium-frequency pulse direct-current negative bias 500V pulse to the workpiece to be plated for 10 minutes to ionize oxygen to generate O+Cleaning by ion bombardmentDepositing the surface of the workpiece;
third, coating process
(1) Maintaining the vacuum degree in the vacuum cavity at 2 × 10-3Pa, closing the upper baffle of the crucible, and pre-melting the metal hafnium film material until the granular metal hafnium is melted into a liquid state;
(2) oxygenating the vacuum chamber to maintain the vacuum degree of the vacuum chamber at 1 × 10-2Pa, opening a baffle on the upper layer of the crucible, adjusting the pulse negative bias voltage applied to the crucible to 100V, opening an electron gun, adjusting the voltage to 8kV, adjusting the current to 0.2A, adjusting the spot size of an electron beam irradiated on the surface of hafnium to a proper size, evaporating the molten hafnium, ionizing the evaporated hafnium vapor and oxygen to form mixed plasma, and depositing the mixed plasma on the surface of a workpiece after rising to form a hafnium oxide film layer;
(3) pulse negative bias on a workpiece table is maintained at 50V, and charged particles are attracted to bombard the workpiece under the action of an electric field, so that the structure of the hafnium oxide film layer is more compact.
Further, the oxygen in the first step is oxygen with a purity of 99.9%.
Furthermore, a tripolar low-pressure reaction ion plating device is used, which comprises a workpiece table, a clamp, an evaporation crucible, a pulse direct current power supply, a tungsten filament, a direct current power supply and an air inlet.
Compared with the prior art, the method provided by the invention overcomes the problem of film material sputtering when the hafnium oxide film is plated by the traditional electron beam evaporation process, and provides a method for preparing the hafnium oxide film by using a three-stage low-pressure reactive ion plating method, so that the node defect probability possibly occurring during deposition of the hafnium oxide film is reduced, and the laser damage threshold of the film is improved.
The hafnium metal is adopted to replace hafnium oxide to serve as a film material, and as the hafnium metal has good fluidity after being melted, when electron beam evaporation is adopted, internal bubbles are easy to discharge, the phase change volume of the hafnium oxide is not changed, and the like, so that the number of sources (seeds) of the nodule defects is greatly reduced. Applying DC bias voltage to the electron beam crucible to ionize hafnium metal vapor evaporated from the crucible and oxygen introduced into the vacuum chamberPlasma (cloud). A tungsten filament connected with direct current is transversely arranged above the electronic gun crucible and used for emitting thermal electrons to increase the ionization rate of the gas. Applying pulsed DC negative bias to the workpiece stage to attract the positively charged Hf+And O+And bombarding the film layer to densify the structure.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a three-pole low-pressure reactive ion plating apparatus.
FIG. 1 depicts the following:
1 is a pulse direct current power supply, 2 is a workpiece table and a clamp, 3 is generated plasma cloud, 4 is a tungsten filament and a direct current power supply, 5 is an evaporation crucible, 6 is an air inlet, and 7 is a pulse direct current power supply.
Detailed Description
For the purpose of promoting a clear understanding of the objects, aspects and advantages of the embodiments of the invention, reference will now be made to the drawings and detailed description, wherein there are shown in the drawings and described in detail, various modifications of the embodiments described herein, and other embodiments of the invention will be apparent to those skilled in the art.
The exemplary embodiments of the present invention and the description thereof are provided to explain the present invention and not to limit the present invention. Additionally, the same or similar numbered elements/components used in the drawings and the embodiments are used to represent the same or similar parts.
As used herein, the terms "first," "second," …, etc., do not denote any order or sequence, nor are they used to limit the present invention, but rather are used to distinguish one element from another or from another element or operation described in the same technical language.
With respect to directional terminology used herein, for example: up, down, left, right, front or rear, etc., are simply directions with reference to the drawings. Accordingly, the directional terminology used is intended to be illustrative and is not intended to be limiting of the present teachings.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
As used herein, "and/or" includes any and all combinations of the described items.
As used herein, the terms "substantially", "about" and the like are used to modify any slight variation in quantity or error that does not alter the nature of the variation. Generally, the range of slight variations or errors modified by such terms may be 20% in some embodiments, 10% in some embodiments, 5% in some embodiments, or other values. It should be understood by those skilled in the art that the aforementioned values can be adjusted according to actual needs, and are not limited thereto.
Certain words used to describe the present application are discussed below or elsewhere in this specification to provide additional guidance to those skilled in the art in describing the present application.
The invention comprises the following steps: a method for preparing a hafnium oxide thin film comprises the following steps:
first, preparation of workpiece to be plated
Placing a workpiece to be plated in acetone and isopropanol solutions in sequence, performing ultrasonic cleaning for 10 minutes respectively, and then drying the workpiece by using dry argon to remove oil stains, impurities and the like attached to the surface of the workpiece to be plated;
secondly, ion cleaning and activation of the workpiece to be plated
(1) Placing the processed workpiece to be plated on a rotary base body table in a vacuum chamber for fixing, and vacuumizing the cavity of the vacuum chamber to 2 x 10-3Introducing high-purity oxygen (with the purity of 99.9%) after Pa, and maintaining the pressure of the vacuum chamber at 3 Pa;
(2) opening a workpiece table biasing device, and applying intermediate frequency to the workpiece to be platedPulsed DC negatively biased 500V pulses (250kHz frequency, 40% duty cycle) for 10 minutes to ionize oxygen to produce O+Cleaning the surface of the workpiece to be deposited by ion bombardment;
third, coating process
(1) Maintaining the vacuum degree in the vacuum cavity at 2 × 10-3Pa, closing the upper baffle of the crucible, and pre-melting the metal hafnium film material until the granular metal hafnium is melted into a liquid state;
(2) oxygenating the vacuum chamber to maintain the vacuum degree of the vacuum chamber at 1 × 10-2Pa, opening a baffle on the upper layer of the crucible, adjusting the pulse negative bias voltage applied to the crucible to 100V, opening an electron gun, adjusting the voltage to 8kV, adjusting the current to 0.2A, adjusting the spot size of an electron beam irradiated on the surface of hafnium to a proper size, evaporating the molten hafnium, ionizing the evaporated hafnium vapor and oxygen to form mixed plasma, and depositing the mixed plasma on the surface of a workpiece after rising to form a hafnium oxide film layer;
(3) pulse negative bias on the workpiece table is maintained at 50V, and charged particles are attracted to bombard the workpiece by the action of an electric field, so that the structure of the hafnium oxide film layer is more compact.
The method overcomes the problem of film material sputtering when the hafnium oxide film is plated by the traditional electron beam evaporation process, and provides the method for preparing the hafnium oxide film by using the tripolar low-pressure reactive ion plating method, so that the node defect probability possibly occurring during deposition of the hafnium oxide film is reduced, and the laser damage threshold of the film is improved.
In another aspect, as shown in fig. 1, the present invention comprises a tripolar low-pressure reactive ion plating apparatus, comprising 1 a pulsed dc power supply, 2a workpiece stage and a jig, 3 a generated plasma cloud, 4 a tungsten filament and a dc power supply, 5 an evaporation crucible, 6 an air inlet, and 7 a pulsed dc power supply.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. A method for preparing a hafnium oxide thin film is characterized by comprising the following steps:
first, preparation of workpiece to be plated
Placing a workpiece to be plated in acetone and isopropanol solutions in sequence, performing ultrasonic cleaning for 10 minutes respectively, and then drying the workpiece by using dry argon to remove oil stains, impurities and the like attached to the surface of the workpiece to be plated;
secondly, ion cleaning and activation of the workpiece to be plated
(1) Placing the processed workpiece to be plated on a rotary base body table in a vacuum chamber for fixing, and vacuumizing the cavity of the vacuum chamber to 2 x 10-3Introducing oxygen after Pa, and maintaining the pressure of the vacuum chamber at 3 Pa;
(2) opening the workpiece table bias device, applying medium-frequency pulse direct-current negative bias 500V pulse to the workpiece to be plated for 10 minutes to ionize oxygen to generate O+Cleaning the surface of the workpiece to be deposited by ion bombardment;
third, coating process
(1) Maintaining the vacuum degree in the vacuum cavity at 2 × 10-3Pa, closing the upper baffle of the crucible, and pre-melting the metal hafnium film material until the granular metal hafnium is melted into a liquid state;
(2) oxygenating the vacuum chamber to maintain the vacuum degree of the vacuum chamber at 1 × 10-2Pa, opening a baffle on the upper layer of the crucible, adjusting the pulse negative bias voltage applied to the crucible to 100V, opening an electron gun, adjusting the voltage to 8kV and the current to 0.2A, adjusting the spot size of an electron beam irradiated on the surface of hafnium, evaporating the hafnium in a molten state, ionizing the evaporated hafnium vapor and oxygen to form mixed plasma, and depositing the mixed plasma on the surface of a workpiece after rising to form a hafnium oxide film layer;
(3) pulse negative bias on the workpiece table is maintained at 50V, and charged particles are attracted to bombard the workpiece by the action of an electric field, so that the structure of the hafnium oxide film layer is more compact.
2. The method according to claim 1, wherein the hafnium oxide thin film is prepared by: the purity of the oxygen was 99.9%.
3. A preparation method of a hafnium oxide film is characterized in that a tripolar low-pressure reaction ion plating device is used, wherein the device comprises a workpiece table, a clamp, an evaporation crucible, a pulse direct current power supply, a tungsten filament, a direct current power supply and an air inlet.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011206543.0A CN114438458A (en) | 2020-11-03 | 2020-11-03 | Preparation method of hafnium oxide film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011206543.0A CN114438458A (en) | 2020-11-03 | 2020-11-03 | Preparation method of hafnium oxide film |
Publications (1)
Publication Number | Publication Date |
---|---|
CN114438458A true CN114438458A (en) | 2022-05-06 |
Family
ID=81361798
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202011206543.0A Pending CN114438458A (en) | 2020-11-03 | 2020-11-03 | Preparation method of hafnium oxide film |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114438458A (en) |
-
2020
- 2020-11-03 CN CN202011206543.0A patent/CN114438458A/en active Pending
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US20090200158A1 (en) | High power impulse magnetron sputtering vapour deposition | |
US20110011737A1 (en) | High-power pulse magnetron sputtering apparatus and surface treatment apparatus using the same | |
US20040089535A1 (en) | Process and apparatus for pulsed dc magnetron reactive sputtering of thin film coatings on large substrates using smaller sputter cathodes | |
CN111088472A (en) | Coating system | |
CN103469164B (en) | Device and method for realizing plasma activation electron beam physical vapor deposition | |
US6296743B1 (en) | Apparatus for DC reactive plasma vapor deposition of an electrically insulating material using a shielded secondary anode | |
CN114438458A (en) | Preparation method of hafnium oxide film | |
CN114540779B (en) | Composite cathode, magnetron sputtering coating equipment and coating method | |
Oskomov et al. | Investigation of plasma ion composition generated by high-power impulse magnetron sputtering (HiPIMS) of graphite | |
CN102732889B (en) | Method and apparatus for removing metal on wafer clamp | |
JP2002306957A (en) | Plasma treating device | |
KR20190119274A (en) | Sputter gun and sputtering deposition apparatus having the same | |
CN114318280B (en) | Method for measuring and controlling nanocluster growth | |
Azuma et al. | Electrical and optical characteristics of high-power pulsed sputtering glow discharge | |
JPS63458A (en) | Vacuum arc vapor deposition device | |
CN115058692B (en) | Preparation method of target film of neutron tube target | |
JPH02156066A (en) | Method for cleaning base material | |
KR930008340B1 (en) | Sputtering device | |
JPH04276062A (en) | Arc deposition device | |
RU2023742C1 (en) | Method of applying protective, decorative and wear-restant coatings | |
JPS63303050A (en) | Manufacture of thin zircon nitride film | |
KR100701365B1 (en) | Apparatus for improving sputtering effect according to plasma source in pvd | |
KR100295617B1 (en) | High vacuum magnetron sputtering method | |
KR100237166B1 (en) | The method for tin coating using ion beam | |
JP6569900B2 (en) | Sputtering apparatus and film forming method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
DD01 | Delivery of document by public notice |
Addressee: Xue Yapeng Document name: Notice of publication of patent application for invention |
|
DD01 | Delivery of document by public notice | ||
DD01 | Delivery of document by public notice |
Addressee: Xue Yapeng Document name: Notification before the expiration of the request period for substantive examination of an invention patent application |
|
DD01 | Delivery of document by public notice | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20220506 |