CN112053929A - Component for plasma chamber interior and method of making same - Google Patents
Component for plasma chamber interior and method of making same Download PDFInfo
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- CN112053929A CN112053929A CN201910489962.0A CN201910489962A CN112053929A CN 112053929 A CN112053929 A CN 112053929A CN 201910489962 A CN201910489962 A CN 201910489962A CN 112053929 A CN112053929 A CN 112053929A
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- 238000000034 method Methods 0.000 claims abstract description 70
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- 229910052731 fluorine Inorganic materials 0.000 claims description 25
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- 239000000758 substrate Substances 0.000 claims description 22
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 17
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- 238000005240 physical vapour deposition Methods 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 15
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- 238000010884 ion-beam technique Methods 0.000 claims description 14
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 12
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 11
- 229910052727 yttrium Inorganic materials 0.000 claims description 10
- 238000000151 deposition Methods 0.000 claims description 7
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical group [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 3
- 229910052765 Lutetium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 229910052775 Thulium Inorganic materials 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229910052706 scandium Inorganic materials 0.000 claims description 3
- 230000005684 electric field Effects 0.000 claims description 2
- 238000005530 etching Methods 0.000 abstract description 25
- 238000001020 plasma etching Methods 0.000 abstract description 9
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- CHBIYWIUHAZZNR-UHFFFAOYSA-N [Y].FOF Chemical compound [Y].FOF CHBIYWIUHAZZNR-UHFFFAOYSA-N 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 230000008020 evaporation Effects 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 8
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 8
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- 150000002367 halogens Chemical class 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32458—Vessel
- H01J37/32477—Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings
- H01J37/32495—Means for protecting the vessel against plasma
-
- 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/32—Processing objects by plasma generation
- H01J2237/33—Processing objects by plasma generation characterised by the type of processing
- H01J2237/334—Etching
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Analytical Chemistry (AREA)
- Drying Of Semiconductors (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The application provides a component used in a plasma chamber and a manufacturing method thereof, wherein the component in the plasma chamber is provided with a coating, the coating comprises oxyfluoride of rare earth elements, and the chemical formula is RexOyFz(x ≠ 0, y ≠ 0, z ≠ 0), wherein Re is a rare earth element, and RexOyFzIs in a crystalline phase. Because its structure is crystalline phase, has specific structure for the coating has certain structural stability, in the in-service process, can keep structural stability, thereby reduces the coating fracture risk, can keep the stability of cavity etching environment. In addition, the rare earth oxyfluoride is used as a protective material of the plasma etching cavity, so that different etching processes can be met, such as simultaneous CF (compact flash) resistance4And O2The plasma etching requirement is wider in application range, continuous production efficiency can be improved, and parts do not need to be replaced frequently, so that production cost can be reduced.
Description
Technical Field
The invention relates to the technical field of plasma processing, in particular to a component used in a plasma chamber and a manufacturing method thereof.
Background
Plasma etching processes play a major role in the field of semiconductor device fabrication, and require relatively high corrosion resistance for components inside a plasma chamber, which are often in a corrosive environment. In order to better protect the components inside the plasma chamber and prevent the components inside the plasma chamber from being corroded by plasma in the long-term use process, researchers have proposed that the components inside the plasma chamber can be protected by yttrium fluoride or yttrium oxide coating, and a good plasma corrosion resistant effect can be achieved.
However, as semiconductor high-end processes (below 10 ×) continue to develop, the plasma etching process imposes a severe requirement on the stability of the etching chamber environment. All the components in contact with the plasma therefore require: 1. high surface compactness and resistance to CF4And/or O2The plasma is corroded, the material structure is not changed as much as possible, and the stability of the cavity etching environment is kept. 2. The initialization time of the etching machine is shortened, the service life of the component is prolonged, the replacement frequency of the component is reduced, and the recovery time after cavity maintenance is shortened.
Aiming at the requirements, the protection effect of yttrium oxide and yttrium fluoride is limited, and the actual requirements cannot be met, so how to provide a novel high-density high-CF-resistance high-service-life long-service-life component4And/or O2Plasma etching, a coating material that maintains the stability of the chamber etching environment, is the target of further research.
Disclosure of Invention
In view of the above, the present invention provides a component for plasma chamber interior and a method for manufacturing the same, so as to solve the problem that the coating in the prior art cannot satisfy the CF resistance at the same time4And/or O2Plasma corrosion, the stability requirement of the etching environment of the cavity is maintained.
In order to achieve the purpose, the invention provides the following technical scheme:
a component inside a plasma chamber, comprising:
a component body within the plasma chamber;
a coating on the component body;
wherein the coating comprises rare earth oxyfluoride having the chemical formula RexOyFz(x ≠ 0, y ≠ 0, z ≠ 0), wherein Re is a rare earth element, and RexOyFzIs in a crystalline phase.
Preferably, the coating further comprises an oxide of the rare earth element and/or a fluoride of the rare earth element.
Preferably, the rare earth element is yttrium element, and the oxide of the rare earth element is Y2O3The fluoride of the rare earth element is YF3。
Preferably, the crystalline phase is a tetragonal phase, a cubic phase or a rhombohedral structure.
Preferably, the coating has a thickness in the range of 0.001 μm to 100um, inclusive.
Preferably, the rare earth element is at least one of Y, Sc, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu.
Preferably, the component body comprises: at least one of a cover plate, a gasket, a nozzle, a gas distribution plate, a showerhead, an electrostatic chuck assembly, a substrate holding frame, a process kit, and a ceramic gasket.
The invention also provides a method of manufacturing a component inside a plasma chamber for forming the above-described component, the method comprising:
the coating is formed on the component body inside the plasma chamber using a plasma enhanced physical vapor deposition process.
Preferably, the forming the coating on the component body inside the plasma chamber by using the plasma enhanced physical vapor deposition process specifically includes:
placing a solid source material in a vacuum reaction chamber;
placing a component body inside a plasma chamber over the solid source material;
arranging an electron gun to evaporate or sputter the solid source material, wherein when the solid source material is evaporated into atoms, molecules and free radicals of gas source materials, the atoms, molecules and free radicals of the gas source materials drift towards the component and are condensed on the surface of the component body;
injecting a first gas into the vacuum reaction cavity, wherein the atoms, molecules and free radicals of the gas source material are ionized by plasma or ion beams dissociated by the first gas to form elements with compact structures and random crystal orientations;
the elements are deposited on the surface of the component body to form the coating.
Preferably, the first gas is a reactive gas, and the plasma or ion beam dissociated by the reactive gas reacts with the atoms, molecules, and radicals to form a dense structure and have randomly oriented crystal elements.
Preferably, the solid source material comprises an oxyfluoride of a rare earth element.
Preferably, the solid source material further comprises an oxide of the rare earth element and a fluoride of the rare earth element.
Preferably, the manufacturing method further comprises:
and injecting a second gas into the vacuum reaction chamber, wherein the second gas is used for reacting with the atoms, the molecules and the free radicals to form a compound containing a rare earth element, an oxygen element and a fluorine element.
Preferably, the solid source material comprises a fluoride of a rare earth element and the second gas is oxygen.
Preferably, the solid source material further comprises an oxyfluoride of the rare earth element.
Preferably, the solid source material comprises an oxide of a rare earth element and the second gas is fluorine gas.
Preferably, the solid source material further comprises an oxyfluoride of the rare earth element.
According to the technical scheme, the upper part of the inner part of the plasma chamber provided by the invention comprises the partA component body and a dense coating disposed on the component body, the coating comprising an oxyfluoride of a rare earth element having a chemical formula RexOyFz(x ≠ 0, y ≠ 0, z ≠ 0), wherein Re is a rare earth element, and RexOyFzIs in a crystalline phase. The rare earth oxyfluoride provided by the invention has a specific crystal structure due to the crystal phase structure, so that the coating has certain structural stability, and the structural stability of the coating can be maintained in the service process, thereby reducing the cracking risk of the coating and maintaining the stability of the cavity etching environment. In addition, the rare earth oxyfluoride serving as a protective material of the plasma etching cavity can meet different etching processes, such as simultaneous CF (compact flash) resistance4And O2Plasma body corrosion's demand, it is wider than single yttria coating or yttrium fluoride coating application scope, moreover, because rare earth element's oxyfluoride has higher stability, can prolong the life of plasma cavity internal part, improves continuous production efficiency, owing to need not often to change the part to can also reduction in production cost.
The invention also provides a method for manufacturing the component in the plasma chamber, which adopts the plasma enhanced physical vapor deposition process to form the coating, so that the coating has a stable crystal phase structure, has high compactness, avoids the influence of particle pollutants introduced in the coating forming process, is oxyfluoride of rare earth elements, contains fluorine elements and oxygen elements, has more stable corrosion resistance to halogen plasma than yttrium oxide, and has O resistance2The plasma is more stable in corrosion resistance than yttrium fluoride, so that the rare earth oxyfluoride is more suitable for etching the protective material of the inner wall of the cavity.
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 embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of a PECVD apparatus according to an embodiment of the present invention;
FIGS. 2-7 are schematic diagrams of a plasma enhanced physical vapor deposition process for forming a yttrium oxyfluoride coating according to an embodiment of the present invention;
FIG. 8 is a surface topography of a yttrium oxyfluoride coating provided in an embodiment of the present invention;
FIG. 9 is a longitudinal sectional view of a yttrium oxyfluoride coating provided in accordance with an embodiment of the present invention.
Detailed Description
As mentioned in the background section, the prior art yttrium oxide and yttrium fluoride have limited protective effects and do not meet practical requirements, particularly not simultaneously resist CF4And O2And (5) plasma etching.
The inventors have discovered that maintaining the stability of the plasma etch process chamber environment is one of the major challenges in advanced integrated circuit manufacturing. On one hand, when the polysilicon etching and the metal etching are finished by the plasma, the inner wall of the cavity body is corroded by the plasma, and a certain metal pollution is brought to the wafer etching due to insufficient protection; on the other hand, a by-product (CF) of plasma etching a waferxPolymer of (b) adheres to the inner wall of the chamber, and the gradual accumulation affects the thickness of the sheath layer of the plasma, resulting in the phenomena of etch rate decrease and drift.
Yttria (Y) due to chemical and physical stability2O3) Coatings have been shown to protect surfaces of etching devices or chamber components exposed to halogen-containing plasmas, resulting in good plasma resistance. However, it has been found in practice that as the number of wafers processed increases, Y permeates due to fluorine or chlorine gas2O3The oxygen contained therein is gradually replaced by fluorine or chlorine in the processing gas, Y2O3Micro particles corroded to YOF, YCl or YOCl are accumulated and finally fall on the etched wafer to cause particle pollution and influenceThe process stability of the process. For this reason, these parts must be replaced at intervals to restore the stability of etching in actual production. The shut down/replacement/recovery operation substantially increases the cost of production significantly, reducing the efficiency of continuous production.
In order to solve the problem of poor halogen plasma corrosion resistance of the yttrium oxide coating, yttrium oxide is fluorinated or yttrium fluoride is used to replace the yttrium oxide coating in the prior art, so that the inner wall of an etching cavity is protected. Wherein the fluorination comprises exposing the coated surface to a plasma of a fluorine-containing species (e.g., at a density of about 1X 10)9e-/cm3Intermediate CF4Plasma or CF3/CF4Plasma) for a sufficient time to fluorinate the surface of the coating to form a YOF film and improve the corrosion resistance of the device to halogen plasma. For YF3On the one hand, the halogen corrosion resistance is improved and Y2O3The comparison is not obvious, but on the other hand it is for the treatment of O-containing materials2YF in plasma process3It is oxidized and thus is not widely used in practice.
Furthermore, the inventors have found that in the prior art, yttrium oxide is fluorinated to YOF by long-term fluorination or yttrium fluoride is oxidized to YOF by oxidation, and YOF formed in either way has a composition of Y2O3And YF3The mixture of (a) and, in addition, the existing oxidation or fluorination techniques, are liable to cause cracking of the original coating. This is due to Y2O3And YF3The volume of the crystal cell is not consistent, and the fluorination or oxidation process causes the generation of compressive stress or tensile stress in the coating, so that the coating is easy to crack, further the protective function of the coating is damaged, and the problems of particle pollution, even metal pollution and the like of an etching chamber are caused.
Specifically, the existing fluorination or oxidation technology is unstable in composition and structure of the coating, and is easy to cause the performance drift of the etching cavity: y is2O3And YF3The fluorination or oxidation process of (2) is a long-term diffusion process, and the concentration of O or F on the surface of the coating is always higher than that in the coating, so that the surface of the coating always existsIn the concentration gradient of O or F, diffusion exists all the time, fluorination or oxidation processes occur all the time, the chemical environment of the boundary of the etching cavity is unstable, and the performance of the etching cavity drifts.
Based on this, the present invention provides a component inside a plasma chamber, comprising:
a component body within the plasma chamber;
a coating on the component body;
wherein the coating comprises rare earth oxyfluoride having the chemical formula RexOyFz(x ≠ 0, y ≠ 0, z ≠ 0), wherein Re is a rare earth element, and RexOyFzIs in a crystalline phase.
The coating on the component in the plasma cavity provided by the invention is the oxyfluoride of the rare earth element, the structure of the coating is a crystalline phase, and the coating has a specific structure, so that the coating has certain stability, the structural stability is maintained in the service process, and the cracking risk of the coating is reduced. Moreover, the oxyfluoride of the rare earth element contains oxygen element and fluorine element, has the characteristic of high compactness (close to 100 percent of theoretical density), can reduce the diffusion process of F or O in the coating and effectively protects components in the plasma chamber.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In one embodiment of the invention, a component inside a plasma chamber is provided, comprising: a component body within the plasma chamber; a coating on the component body; wherein the coating comprises rare earth oxyfluoride having the chemical formula RexOyFz(x ≠ 0, y ≠ 0, z ≠ 0), wherein Re is a rare earth element, and RexOyFzIs in a crystalline phase.
It should be noted that, in order to increase the concentration of F or O in the coating, eliminate the concentration gradient of the boundary layer, and maintain the stability of the boundary environment of the etching chamber. In other embodiments of the present invention, the coating may further include an oxide of the rare earth element or a fluoride of the rare earth element.
The specific elements of the rare earth elements are not limited in the embodiment of the invention, and the rare earth elements can be one or more of Y, Sc, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu. It should be noted that, in the prior art, in consideration of cost issues and industrial application effects, the rare earth element often used is yttrium element, that is, the material of the coating in the embodiment of the present invention is YOF of crystalline phase, but with the development of the industry, oxyfluoride of other rare earth elements may also be applied, and as atomic molar mass of other rare earth elements is larger, the plasma etching resistance effect is expected to be better and more stable.
In the present embodiment, when the rare earth element is an yttrium element, the crystal phase may include a rhombohedral, cubic phase, or tetragonal YOF phase. The rare earth oxyfluoride may have a chemical composition including YOF and Y5O4F7、Y7O6F9YOF having a single phase or the like, and Y2O3、YF3A mixture of (a). I.e. the composition of the coating may also comprise oxides of rare earth elements and/or fluorides of rare earth elements. It should be noted that the mixture described in this embodiment refers to a mixture including both the rare earth oxyfluoride and the rare earth oxide and/or the rare earth fluoride in the single-layer structure of the coating, and is not a layered structure of the rare earth oxyfluoride and the rare earth oxide and/or the rare earth fluoride.
In addition, when the rare earth element is a rare earth element other than yttrium element, the corresponding crystal phase is a crystal phase in which the corresponding rare earth element is bonded to oxygen element and fluorine element, and this will not be described in detail in this example. The rare earth oxyfluoride formed by any rare earth element, oxygen element and fluorine element has the characteristic of high compactness (close to 100% of theoretical density), so that the diffusion process of F or O in a coating can be reduced, and the structure of the internal part of the plasma chamber is effectively protected.
It is noted that prior art YOF, such as spray YOF, contain 3% -5% of pores, so 100-200 μm thick is required to prevent plasma from eroding the substrate (usually aluminum or ceramic) through these pores. However, because of the high compactness of the material coated by the method of the invention, the thickness of the coating can be reduced, the thickness is not required to be large in the practical use process, the thickness can range from 0.001 μm to 100 μm according to the practical requirement, the end value is included, and the thickness can be typically more than 10 μm and less than 60 μm, and the thinner coating can prevent parts exposed to plasma from being corroded.
High-frequency radio frequency power (more than 13MHz) and low-frequency radio frequency power (less than or equal to 2MHz) are usually applied to the plasma reaction cavity at the same time, and for the high-frequency radio frequency power, although the part surface coating YOF in the reaction cavity is an insulating material, the thickness of 100-. However, for low frequency rf power, the thickness of the surface coating significantly affects the rf power penetration, i.e., the thicker the coating, the harder the rf power penetration. When the plasma corrosion resistant material layer is coated on the parts such as the liner, the gas spray header, the conductive base, the inner wall of the reaction cavity and the like in the plasma processing cavity, if the coating material is too thick, the low-frequency radio frequency power cannot be effectively coupled to the parts needing coupling. The coating method can obtain a stable enough corrosion-resistant material layer YOF, and the material layer is compact and thin, so that low-frequency radio frequency power can be efficiently coupled between different parts coated with the coating. In addition, according to the contents of F and O in the manufacturing process, the heights of F and O in the coating and the thickness of the coating can be correspondingly designed, and the long-life service of the etching cavity component is realized.
The embodiments of the present invention do not limit which specific structures the components inside the plasma chamber include, and optionally, each component for releasing plasma in the plasma chamber includes: at least one of a cover plate, a gasket, a nozzle, a gas distribution plate, a showerhead, an electrostatic chuck assembly, a substrate holding frame, a process kit, a ceramic gasket, and the like.
In this example, in order to obtain the rare earth oxyfluoride having high density and a crystal phase, it was possible to achieve the high density by an enhanced PVD method, a plasma enhanced method or an ion beam enhanced method.
Specifically, in one exemplary process, a Plasma Enhanced Physical Vapor Deposition (PEPVD) process is utilized to produce an enhanced yttrium oxyfluoride coating having a good/dense grain structure and random crystal orientation (random crystal orientation), e.g., based on Y5O4F7、Y7O6F9The coating of (1), wherein (1) the deposition is performed in a low pressure or vacuum chamber environment; (2) at least one deposition element or component is evaporated or sputtered from a material source, the evaporated or sputtered material concentrating on the substrate surface (this part of the process is a physical process and is referred to herein as the physical vapor deposition or PVD part); (3) simultaneously, one or more plasma sources are used to emit ions or generate a plasma to surround the substrate surface, at least one deposited element or component being ionized and reacting with the evaporated or sputtered element or component in the plasma or on the substrate surface; (4) the substrate is coupled to a negative voltage so that it is bombarded by ionized atoms or ions during the deposition process. The reactions in (3) and (4) refer to the "plasma enhanced" (or PE) function in PEPVD.
It should be noted that the plasma source may be used (1) to ionize, decompose, and excite reactive gases to enable deposition processes to be performed at low substrate temperatures and high coating growth rates (as the plasma generates more ions and radicals), or (2) to generate energetic ions (energetic ions) for the substrate to cause the ions to bombard the substrate surface and help form thick and concentrated coatings thereon. More particularly, the plasma source is used to alternatively or collectively perform functions (1) and/or (2) to form a coating on a substrate. This combination of coatings having sufficient thickness and compactness is referred to herein as "enhanced coatings" (hereinafter: A coatings).
Unlike conventional plasma spray processes, where the coating is deposited in an atmospheric environment (atmospheric environment), the enhanced coating provided by the present invention is deposited in a low pressure or vacuum environment. Also, while conventional plasma spray processes deposit coatings using small powder particles, the enhanced coatings of the present invention deposit by condensation of atomic radicals (atoms) or particulates on the surface of the material. The coating properties thus obtained differ from those of the prior art coatings, even when materials of the same composition are used. For example, the yttrium oxyfluoride coating obtained according to one embodiment of the invention is substantially non-porous, has a surface roughness of better than 1 μm, and has a higher etch resistance than the YOF coating obtained with the prior art Plasma Spray (PS).
Specific embodiments of the present invention will be described below with reference to the accompanying drawings. First, an apparatus and method for depositing an enhanced coating is described. FIG. 1 illustrates an apparatus for depositing an enhanced coating according to one embodiment of the present invention. The apparatus employs a process known as PEPVD to deposit enhanced coatings, where PE and PVD components are shown in dashed lines in fig. 1. Traditionally, Chemical Vapor Deposition (CVD) or Plasma Enhanced Chemical Vapor Deposition (PECVD) refers to a chemical process in which a substrate is exposed to one or more volatile precursors (volatile precursors) that react or decompose at the substrate surface to produce the desired deposited film on the substrate surface. Additionally, PVD refers to a coating process that involves purely physical processes that condense a desired thin film material, usually a solid source substance, that is vaporized or sputtered, to deposit a thin film on the surface of a substrate. Thus, it can be appreciated that the aforementioned PEPVD is a hybrid of these two processes. That is, the PEPVD includes condensation of atoms, radicals, or molecules belonging to a physical process (PVD part) and plasma chemical reaction (PE part) performed in the chamber and on the surface of the substrate.
In fig. 1, the chamber 100 is evacuated by a vacuum pump 115. The component to be coated, i.e. the component body 110, is coated, in this embodiment a gas shower, a focus ring, a cover ring, a confinement ring, etc., is attached to the support ring 105. And, a negative bias is applied to the member to be coated 110 through the support ring 105.
A source material 120 includes the component to be deposited, which is typically in solid form. For example, if the film to be deposited is YOF, the solid source material 120 should include yttrium (or fluorine, or oxygen), possibly along with other materials, such as oxygen, fluorine (or yttrium), and the like. To form the physical deposit, the solid source material is evaporated or sputtered. In the embodiment shown in fig. 1, evaporation is performed using an electron gun (electron gun)125, which directs an electron beam (electron beam)130 over the solid source material 120. When the solid source material is vaporized to form source material atoms, molecules, or radicals, the source material atoms, molecules, or radicals drift toward the component body 110 and condense on the component body 110, as shown by the dashed arrows.
The plasma enhanced component consists of a gas injector (gas injector)135 that injects an active or inactive source gas, such as a gas containing argon, oxygen, fluorine, into the chamber 100, shown in phantom. At least one pair of electrodes is provided in the gas injector 135, and a high voltage is applied to the electrodes so that the gas flowing therethrough is ionized by the high voltage to form a plasma, which is injected into the chamber 100 by the gas injector 135. Plasma is maintained in the space beneath the component body 110, and the electromagnetic field, which in this embodiment is illustratively generated by a coil 145 coupled to an rf source 150, causes ions in the plasma 140 to be driven in a circular motion by the electric field, such that ions beneath the component body 110 are accelerated and maintained at a sufficient concentration. Without being bound by theory, several processes occur in the PE part. First, a non-reactive ionized gas component, such as argon, bombards the body 110 of the part, as it is being accumulated, thereby densifying the film. The effect of ion bombardment results from a negative bias applied to the component body 110 and the support ring 105, or from ions emitted by the plasma source and directed at the component body 110. In addition, reactive gas species or radicals, such as oxygen or fluorine, react with the vaporized or sputtered source material, either on the surface of the component body 110 or within the chamber. Thus, the above processes have physical processes (bombardment and coagulation) and chemical processes (e.g., oxidation and ionization).
That is, in the embodiment of the present invention, the forming the coating on the component body inside the plasma chamber by using the plasma enhanced physical vapor deposition process specifically includes: placing a solid source material in a vacuum reaction chamber; placing a component body inside a plasma chamber over the solid source material; arranging an electron gun to evaporate or sputter the solid source material, wherein when the solid source material is evaporated into atoms, molecules and free radicals of gas source materials, the atoms, molecules and free radicals of the gas source materials drift towards the component and are condensed on the surface of the component body; injecting a first gas into the vacuum reaction cavity, wherein the atoms, molecules and free radicals of the gas source material are ionized by plasma or ion beams dissociated by the first gas to form elements with compact structures and random crystal orientations; the elements are deposited on the surface of the component body to form the coating. Wherein the ionization can enable the elements with compact structures and random crystal orientation to deposit at low substrate temperature and high growth speed to form the coating. Therefore, a highly dense coating layer can be formed by plasma enhancement or ion beam enhancement.
It should be noted that the first gas can be any gas capable of generating plasma, such as Ar, O2，N2And the like, and the embodiments of the present invention are not particularly limited. That is, the first gas may be a reactive gas, such as an inactive gas, and when the first gas is a reactive gas, the plasma or ion beam dissociated by the reactive gas reacts with the atoms, molecules, and radicals to form a dense structure and have random structureElements of crystal orientation.
In one embodiment of the present invention, the solid source material is an oxyfluoride of a rare earth element, which may be an oxyfluoride of a rare earth element having a porous structure, and a dense oxyfluoride coating of a rare earth element having a crystalline phase is formed directly through a plasma enhancement or ion beam enhancement process. The coating can also be a solid source material comprising the oxide of the rare earth element and the fluoride of the rare earth element, and can also be directly formed into a rare earth element oxyfluoride coating with higher compactness and crystalline phase through a plasma enhancement or ion beam enhancement process. In other embodiments of the present invention, injecting a second gas into the vacuum reaction chamber, wherein the second gas is used for reacting with the atoms, the molecules and the free radicals to form a compound containing a rare earth element, an oxygen element and a fluorine element. For example, the solid source material may comprise a fluoride of a rare earth element and the second gas is oxygen, or the raw material may further comprise an oxyfluoride of a rare earth element; alternatively, the solid source material may include an oxide of a rare earth element, and the second gas may be fluorine gas, or may further include an oxyfluoride of a rare earth element.
For the sake of clarity of the process of forming oxyfluoride of rare earth element in this embodiment, the formation of yttrium oxyfluoride is taken as an example in this embodiment.
Referring to fig. 2-7, fig. 2-7 are schematic diagrams of a plasma enhanced physical vapor deposition process for forming a yttrium oxyfluoride coating. As shown in fig. 2, YOF is directly used as an evaporation source, vaporized by thermal evaporation (by electron beam heating or resistance heating or other heating means), and then enhanced by plasma or ion beam to form a highly dense YOF coating on a substrate (i.e., a component in the plasma chamber described in the above embodiment). As shown in FIG. 3, YOF and Y are used as they are2O3And YF3As an evaporation source, the vapor is vaporized by thermal evaporation (realized by electron beam heating or resistance heating or other heating methods), and then is enhanced by plasma or ion beamAfter the reaction, a highly dense YOF coating was formed, and it should be noted that in this example, YOF was used as the evaporation source and Y was increased2O3And YF3Is to increase the content of O and F in the coating without continuing to add Y2O3And YF3Converted into YOF. As shown in FIG. 4, YF is used3As an evaporation source, passing through and reacting with O after being vaporized2And carrying out chemical reaction Y + F + O → YOF, and forming a high-density YOF coating after the strengthening action of plasma or ion beams. As shown in FIG. 5, Y is used2O3As an evaporation source, passing through a gas-liquid separator2And carrying out chemical reaction Y + O + F → YOF, and forming a high-density YOF coating after the strengthening action of plasma or ion beams. As shown in FIG. 6, YOF and Y are used2O3As an evaporation source, and introducing F2As a reaction gas, a high-density YOF coating is formed after the enhancement of plasma or ion beams; as shown in FIG. 7, YOF and YF are used3As an evaporation source, and introducing O2As a reaction gas, a highly dense YOF coating is formed after the strengthening action of plasma or ion beams.
Referring to fig. 8 and 9, fig. 8 and 9 are SEM pictures of the YOF coating formed by the method shown in fig. 2. Wherein FIG. 8 is a surface topography of the coating and FIG. 9 is a longitudinal section of the coating; as seen from fig. 8, the coating surface remained smooth under the condition of magnification of 5000 times, whereas from the SEM picture of longitudinal section shown in fig. 9, the coating had no analogues of pores observed under the condition of magnification of 50000 times, and the surface coating had high denseness.
It should be noted that the conventional yttria fluoride coating is formed by a plasma spray process. The process is characterized in that micron-sized yttrium oxyfluoride particles are sputtered on a workpiece substrate in a semi-molten state by plasma heating in an atmospheric environment, the yttrium oxyfluoride particles are cooled, shrunk in volume and stacked to form a coating with a porous structure, and the porosity is generally 3% -5%.
The yttrium oxyfluoride provided by the embodiment of the invention adopts an enhanced PVD technology to deposit a film in a low-pressure or vacuum environment, so that the influence of impurities in the environment can be effectively reduced. The YOF coating has low synthesis temperature, effectively reduces the influence of internal stress caused by mismatching of thermal expansion coefficients of the substrate and the coating, and avoids the falling of the coating and the substrate. And the YOF coating realizes deposition by condensing nanoscale gas atoms, molecules and free radicals on the surface of the material, and the structure density is 100%. The structure has higher density, and the thickness of the coating is in the level of dozens of microns, so that the plasma corrosion can be effectively prevented, the process time is shortened, and the coating process cost is reduced.
And the coating with a specific structure (such as a cubic phase, a tetragonal phase, a rhombohedral structure and the like) has certain structural stability, so that the structural stability is maintained in the service process, and the cracking risk of the coating is reduced. YOF may also be combined with Y2O3And/or YF3The mixture is formed, the diffusion and corrosion effects of F and/or O on the boundary layer of the coating are reduced, and the stability of the boundary environment of the etching cavity is maintained. The YOF coating is used as a protective material of the etching cavity, and can simultaneously meet different etching processes (CF)4/O2Plasma ratio) than Y alone2O3Coating or YF3The coating has wider application range.
It should be noted that, in the present specification, the embodiments are all described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments may be referred to each other.
It is further noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such article or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in an article or device that comprises the element.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (17)
1. A component inside a plasma chamber, comprising:
a component body within the plasma chamber;
a coating on the component body;
wherein the coating comprises rare earth oxyfluoride having the chemical formula RexOyFz(x ≠ 0, y ≠ 0, z ≠ 0), wherein Re is a rare earth element, and RexOyFzIs in a crystalline phase.
2. A component inside a plasma chamber according to claim 1, wherein the coating further comprises an oxide of the rare earth element and/or a fluoride of the rare earth element.
3. The component for a plasma chamber interior according to claim 2, wherein the rare earth element is yttrium and the oxide of the rare earth element is Y2O3The fluoride of the rare earth element is YF3。
4. A component inside a plasma chamber according to claim 3, wherein the crystalline phase is a tetragonal phase, a cubic phase or a rhombohedral structure.
5. A component inside a plasma chamber according to claim 3, wherein the coating has a thickness in a range of 0.001 μ ι η -100 μ ι η, inclusive.
6. A component inside a plasma chamber according to claim 1, wherein the rare earth element is at least one of Y, Sc, La, Ce, Pr, Nd, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu.
7. A component inside a plasma chamber according to claim 1, wherein the component body comprises: at least one of a cover plate, a gasket, a nozzle, a gas distribution plate, a showerhead, an electrostatic chuck assembly, a substrate holding frame, a process kit, and a ceramic gasket.
8. A method of forming a component inside a plasma chamber, for forming a component as claimed in any one of claims 1 to 7, the method comprising:
the coating is formed on the component body inside the plasma chamber using a plasma enhanced physical vapor deposition process.
9. The method for manufacturing a component inside a plasma chamber according to claim 8, wherein the forming the coating on the component body inside the plasma chamber by using a plasma enhanced physical vapor deposition process specifically comprises:
placing a solid source material in a vacuum reaction chamber;
placing a component body inside a plasma chamber over the solid source material;
arranging an electron gun to evaporate or sputter the solid source material, wherein when the solid source material is evaporated into atoms, molecules and free radicals of gas source materials, the atoms, molecules and free radicals of the gas source materials drift towards the component and are condensed on the surface of the component body to form a deposition material layer;
injecting ionized first gas into the vacuum reaction cavity, wherein ions in the first gas bombard the deposition material layer upwards under the driving of an electric field to form elements with compact structures and random crystal orientations;
the elements are deposited on the surface of the component body to form the coating.
10. The method of claim 9, wherein the first gas is a reactive gas, and wherein the dissociated plasma or ion beam of the reactive gas reacts with atoms, molecules, and radicals of the source material to form a dense structure and random crystallographic orientation of the elements.
11. The method of claim 9, wherein the solid source material comprises an oxyfluoride of a rare earth element.
12. The method of claim 11, wherein the solid source material further comprises an oxide of the rare earth element and a fluoride of the rare earth element.
13. A method of fabricating a component inside a plasma chamber as recited in claim 9, further comprising:
and injecting a second gas into the vacuum reaction cavity, wherein the second gas is used for reacting with the gas source material atoms, molecules and free radicals to form a compound containing a rare earth element, an oxygen element and a fluorine element.
14. A method of fabricating a component inside a plasma chamber as claimed in claim 13, wherein the solid source material comprises a fluoride of a rare earth element and the second gas is oxygen.
15. The method of claim 14, wherein the solid source material further comprises an oxyfluoride of the rare earth element.
16. The method of claim 13, wherein the solid source material comprises an oxide of a rare earth element and the second gas is fluorine gas.
17. The method of claim 16, wherein the solid source material further comprises an oxyfluoride of the rare earth element.
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| TWI768367B (en) | 2022-06-21 |
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Application publication date: 20201208 |