CN116770386A - Preparation method of protective layer on inner wall of chamber - Google Patents
Preparation method of protective layer on inner wall of chamber Download PDFInfo
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- CN116770386A CN116770386A CN202310963147.XA CN202310963147A CN116770386A CN 116770386 A CN116770386 A CN 116770386A CN 202310963147 A CN202310963147 A CN 202310963147A CN 116770386 A CN116770386 A CN 116770386A
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- protective layer
- wall
- chamber
- anodic oxidation
- hard anodic
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
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Abstract
The invention provides a preparation method of a protective layer on the inner wall of a cavity, which comprises the following steps: pretreating the inner wall of the chamber by sand blasting or HF pickling; forming a first protection layer on the inner wall of the chamber by adopting a hard anodic oxidation mode; and depositing a parylene coating on the first protective layer to carry out hole sealing operation on the first protective layer, so as to form a second protective layer to finish the protective layer preparation work of the inner wall of the cavity.
Description
Technical Field
The invention relates to the field of semiconductor process equipment, in particular to a preparation method of a protective layer on the inner wall of a chamber.
Background
In the prior art, cleaning work of a semiconductor process chamber such as a deposition chamber mainly uses fluorine ion dry etching, the actual cleaning time is properly adjusted based on the number of particles and the use requirement of the chamber, and if the cleaning time is improperly set, an over etching phenomenon, such as AlF formation, is easy to occur 3 The particles drop onto the wafer, affecting the yield of the product.
Meanwhile, the current deposition equipment mainly adopts the modes of prefabricating the protective layer before deposition, adding ceramic parts and the like to protect the inner wall of the cavity, but the thickness of the prefabricated protective layer on a part of the area of the inner wall of the cavity is thinner due to the structural complexity of the deposition cavity, so that the prefabricated protective layer is easy to be carved through. In addition, due to the influences of machining tolerance, material thermal expansion and other factors, gaps exist between part of ceramic parts and the inner wall of the chamber, once equipment runs for a long time, the positions are easily severely etched, so that the problem of dropping particulate matters is generated, and the process quality is influenced.
In order to overcome the above-mentioned drawbacks of the prior art, there is a need in the art for a method for preparing a protective layer on an inner wall of a chamber, which is capable of sealing material pores, improving adhesion between layers, improving roughness of the inner wall surface, and further improving usability of semiconductor processing equipment during the process of forming a multi-layer protective layer on the inner wall of the chamber.
Disclosure of Invention
The following presents a simplified summary of one or more aspects in order to provide a basic understanding of such aspects. This summary is not an extensive overview of all contemplated aspects, and is intended to neither identify key or critical elements of all aspects nor delineate the scope of any or all aspects. Its sole purpose is to present some concepts of one or more aspects in a simplified form as a prelude to the more detailed description that is presented later.
In order to overcome the above-mentioned drawbacks of the prior art, the present invention provides a method for preparing a protective layer on an inner wall of a chamber, which may include: pretreating the inner wall of the chamber by sand blasting or HF pickling; forming a first protection layer on the inner wall of the chamber by adopting a hard anodic oxidation mode; and depositing a parylene coating on the first protective layer to carry out hole sealing operation on the first protective layer, so as to form a second protective layer to finish the protective layer preparation work of the inner wall of the cavity.
In one embodiment, preferably, the method for preparing the protective layer may further include: after the second protective layer is formed, the second protective layer is further optimized by oxygen plasma etching or high-frequency laser radiation.
In an embodiment, preferably, the further optimizing the second protective layer by oxygen plasma etching or high frequency laser irradiation may include: the radiation intensity of the high frequency laser radiation is varied to adjust the surface roughness of the second protective layer.
In an embodiment, preferably, the adjusting the surface roughness of the second protection layer may include: the surface roughness Ra value of the second protective layer is controlled to be in the range of 0.025-12.5.
In an embodiment, preferably, the forming the second protection layer may include: the second protective layer is controlled to be compact and nonporous, has uniform thickness and is in the numerical range of 0.01-50 mu m.
In one embodiment, preferably, the forming the first protection layer on the inner wall of the chamber by hard anodic oxidation may include: the hard anodizing process is accomplished using a phosphoric acid electrolyte reaction.
In one embodiment, preferably, the method for preparing the protective layer may further include: after the pretreatment of the inner wall of the chamber by sand blasting or HF pickling is performed, the inner wall of the chamber is cleaned by means of water washing or alkali washing.
In one embodiment, preferably, the method for preparing the protective layer may further include: after the first protective layer is formed on the inner wall of the chamber by adopting a hard anodic oxidation mode, the inner wall of the chamber is cleaned and dried again.
Drawings
The above features and advantages of the present invention will be better understood after reading the detailed description of embodiments of the present disclosure in conjunction with the following drawings. In the drawings, the components are not necessarily to scale and components having similar related features or characteristics may have the same or similar reference numerals.
FIG. 1 is a schematic flow chart of a method for preparing a protective layer on an inner wall of a chamber according to an aspect of the invention; and
fig. 2 is a flow chart of a method for preparing a protective layer on an inner wall of a chamber according to an embodiment of the invention.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present specification, by describing the embodiments of the present invention with specific examples. While the description of the invention will be presented in connection with a preferred embodiment, it is not intended to limit the inventive features to that embodiment. Rather, the purpose of the invention described in connection with the embodiments is to cover other alternatives or modifications, which may be extended by the claims based on the invention.
The following description contains many specific details for the purpose of providing a thorough understanding of the present invention. The invention may be practiced without these specific details. Furthermore, some specific details are omitted from the description in order to avoid obscuring the invention.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
In addition, the terms "upper", "lower", "left", "right", "top", "bottom", "horizontal", "vertical" as used in the following description should be understood as referring to the orientation depicted in this paragraph and the associated drawings. This relative terminology is for convenience only and is not intended to be limiting of the invention as it is described in terms of the apparatus being manufactured or operated in a particular orientation.
It will be understood that, although the terms "first," "second," "third," etc. may be used herein to describe various elements, regions, layers and/or sections, these elements, regions, layers and/or sections should not be limited by these terms and these terms are merely used to distinguish between different elements, regions, layers and/or sections. Accordingly, a first component, region, layer, and/or section discussed below could be termed a second component, region, layer, and/or section without departing from some embodiments of the present invention.
In order to overcome the defects in the prior art, the invention provides a preparation method of a protective layer of the inner wall of a chamber, wherein in the process of forming a multi-layer protective layer on the inner wall of the chamber, pores of materials are closed, adhesiveness between layers is improved, roughness of the surface of the inner wall is improved, and further, the service performance of semiconductor process equipment is improved.
Fig. 1 is a schematic flow chart of a method for preparing a protective layer on an inner wall of a chamber according to an aspect of the invention.
Referring to fig. 1, a method 100 for preparing a protective layer on an inner wall of a chamber according to the present invention may include:
step 101: the chamber inner wall is pretreated by sandblasting or HF pickling.
Further, in an embodiment, preferably, after the pretreatment of the inner wall of the chamber by sand blasting or HF pickling is performed, the inner wall of the chamber may be cleaned by means of water washing or alkali washing.
With continued reference to fig. 1, the method 100 for preparing a protective layer for an inner wall of a chamber according to the present invention may further include:
step 102: and forming a first protection layer on the inner wall of the chamber by adopting a hard anodic oxidation mode.
It should be noted that the material of the first protective layer is not specifically limited, and any material that can be formed by hard anodic oxidation and is suitable for the inner wall of the chamber can be used in the method step of the present invention. For example, preferably, the first protective layer may be an alumina protective layer.
In a preferred embodiment, the hard anodizing process is accomplished using a phosphoric acid electrolyte reaction.
Compared with the prior art that the inner wall protection layer is formed by a common anodic oxidation mode in the deposition chamber, in the embodiment, the preparation method of the protection layer of the inner wall of the chamber is prepared by adopting a phosphoric acid electrolyte reaction mode in the hard anodic oxidation step to form the first protection layer, heavy metal ion wastewater is not generated in the process, harmful gas is not released, and the environment-friendly process production requirement can be met to the greatest extent.
Further, in an embodiment, the method for preparing the protective layer on the inner wall of the chamber provided by the invention further includes: after the first protective layer is formed on the inner wall of the chamber by adopting a hard anodic oxidation mode, the inner wall of the chamber is cleaned and dried again.
With continued reference to fig. 1, the method 100 for preparing a protective layer for an inner wall of a chamber according to the present invention may further include:
step 103: and depositing a parylene coating on the first protective layer to carry out hole sealing operation on the first protective layer, so as to form a second protective layer to finish the preparation work of the protective layer on the inner wall of the cavity.
Parylene (Parylene) is a protective polymer material, chinese name is Parylene, the Parylene can be vapor deposited under vacuum, active molecules of the Parylene have good penetrability, a transparent insulating coating which is free of pinholes and uniform in thickness can be formed in and around the chamber, a complete high-quality protective coating is provided for the inner wall of the chamber, and corrosion of acid, alkali, salt fog, mold and various corrosive gases can be resisted.
It should be noted that, compared with some solutions in the prior art that a multi-layer protection layer is formed for a component in a semiconductor process chamber, the preparation method of the protection layer of the inner wall of the chamber provided by the invention is directed at the whole inner wall of the chamber, including the inner part, the bottom and the periphery of the chamber.
The method provided by the invention can form omnibearing integral protection in the reaction chamber, is corrosion-resistant, simultaneously reduces possible particulate pollution in a plurality of steps of the process flow to the greatest extent, and improves the semiconductor production yield and the service performance of the process equipment chamber to the greatest extent.
In an embodiment of the present invention, the parylene coating may be deposited by normal temperature CVD vapor deposition to form a second protective layer on the basis of the first protective layer formed by hard anodic oxidation.
In particular, in the method for preparing the protective layer on the inner wall of the chamber, the parylene coating is used as a hole sealing material of the first protective layer, and after the first protective layer is deposited by adopting a hard anodic oxidation mode, the hole sealing is carried out by using the parylene coating when the material of the first protective layer is required to be further sealed.
Compared with the prior art, the hole sealing of the hard anodic oxide layer is usually carried out by adopting a way of sealing by boiling water, steam or nickel fluorideThe effect of the parylene coating on sealing the first protective layer material is to ensure that the holes in the first protective layer material formed by hard anodic oxidation are completely sealed, thereby avoiding AlF, for example, in the subsequent deposition process or cleaning process 3 The particles fall into the holes, and then the particles fall onto the wafer from the holes when the subsequent equipment runs for a long time, so that the problem of wafer particles is generated.
Secondly, the parylene coating is used for carrying out hole sealing treatment on the hard anodic oxide layer, the adhesive force between the anodic oxide layer and the parylene coating can be enhanced, the coating is prevented from falling off, a double protective layer is formed, and then the resistance of the inner wall of the chamber to active fluoride ion etching can be improved, and the service life of the chamber is prolonged.
In addition, the parylene coating is deposited to seal the hole to treat the first protective layer, so that the problems that the hole sealing material is not properly selected or is not firmly adhered to the hole sealing material of the anodic oxide layer in the subsequent process can be avoided, the hole sealing material falls onto a wafer, and the problem of wafer particles is caused to influence the yield of process products.
In a preferred embodiment, the method for preparing the protective layer on the inner wall of the chamber provided by the invention further comprises the following steps: after the second protective layer is formed, the second protective layer is further optimized by oxygen plasma etching or high-frequency laser radiation.
The plasma etching method can be reactive plasma (RIE), downstream plasma (downstream), direct plasma (direct plasma), or the like.
More specifically, oxygen plasma etching, typically using O at a pressure in the range of 10 to 1000 Pa 2 Or O 3 The glow discharge of the gas generates molecules or molecular groups capable of carrying out ionic chemical reaction with the film, and the generated reaction products are volatile and can be pumped away in a vacuum chamber with low pressure, thereby realizing etching. By selecting and controlling the composition of the discharge gas, better etch selectivity and higher etch rates can be achieved.
The basic principle of laser radiation etching is to focus a low-power laser beam (such as ultraviolet laser, fiber laser and the like) with high beam quality into a very small light spot, and form very high power density at the focus, so that the material is vaporized and evaporated in an instant, and thus, the expected physical shapes of holes, seams, grooves and the like are formed.
Further, preferably, in an embodiment, the surface roughness of the second protective layer may be adjusted by changing the radiation intensity of the high-frequency laser radiation.
For example, the high-frequency laser radiation can be a continuously adjustable ultrahigh-frequency laser with the frequency ranging from 10kHz to 100kHz, so that a better etching effect can be achieved.
It should be noted that, in this embodiment, the parylene coating is further processed by oxygen plasma etching, such as O2/O3, or high-frequency laser radiation, so as to properly etch the surface of the second protective layer formed by the parylene material, thereby improving the surface roughness of the inner wall of the chamber, and further improving the adhesion between the second protective layer and the front prefabricated protective layer possibly existing in the subsequent deposition process, so as to avoid the problem of dropping of particles caused by improper selection of the hole sealing material of the anodic oxide layer.
In particular, in the preparation method of the protective layer on the inner wall of the chamber, the surface roughness and the coating thickness of the second protective layer formed by the parylene material can be adjusted according to the actual application requirements, so that the parameter requirements of various deposition processes can be met to a large extent.
Further preferably, for example, the surface roughness Ra value of the second protective layer may be controlled to be in the range of 0.025 to 12.5.
It should be noted that, the surface roughness numerical range is only exemplified here, and the purpose is to illustrate the advantage of the preparation method of the protective layer on the inner wall of the chamber provided by the invention, which is controlled by the process, so that the coating has good adhesion. The roughness of materials in different processes is different, in the actual process, the surface roughness of the coating is required to be adjusted according to the granularity performance in the actual process operation process, so that the coating and the prefabricated protective layer are ensured to have good adhesion, and the problem of falling of materials is prevented.
Meanwhile, in a preferred embodiment, the formed second protective layer is compact and nonporous, has uniform thickness and is in a numerical range of 0.01-50 μm, after the coating is added, the shape of the bottom layer is not covered, and the condition that a large amount of coating material in a local area is gathered is avoided, so that the second protective layer is uniform and compact, has a shape retaining effect and is not gathered, and the physical shape of the protective layer is controlled by a process based on the characteristics of the material, so that the second protective layer has excellent etching resistance.
In addition, in the preparation method of the protective layer on the inner wall of the chamber provided by the invention, in the step of forming the hard anodic oxidation protective layer by adopting the phosphoric acid electrolyte for reaction, no heavy metal ion wastewater or harmful gas is released, and the preparation method meets the requirements of green and environment-friendly production process.
In addition, other steps in the preparation method of the protective layer do not generate three wastes, for example, the parylene coating adopted in the formation of the second protective layer does not contain auxiliary agents, and O is adopted in the subsequent treatment of the second protective layer 2 /O 3 In the process of plasma etching or ultrahigh frequency laser radiation, the removed matters escape in the mode of carbon monoxide or carbon dioxide, so that the process effect can be improved, the service performance of process equipment can be improved, and the environment-friendly process production requirement can be met to the greatest extent.
Fig. 2 is a flow chart of a method for preparing a protective layer on an inner wall of a chamber according to an embodiment of the invention.
Referring to fig. 2, in the method for preparing a protective layer on an inner wall of a chamber provided by the present invention, step 201 is performed first, and in this embodiment, the protective layer is prepared on the inner wall of a PECVD chamber.
Step 202 is then performed: the PECVD chamber inner wall is pretreated by adopting a sand blasting or HF pickling mode, so that the surface roughness of the chamber inner wall can be increased, and the adhesion performance of a protective layer formed later can be enhanced.
The following steps are then sequentially performed:
step 203: the inner wall of the chamber is cleaned by adopting a water washing or alkali washing or acid washing mode, so that impurities such as particles and the like generated in the previous link are removed, and the influence on the subsequent process flow is avoided.
Step 204: and forming a first protective layer by hard anodic oxidation. More specifically, it is preferred that the hard anodizing step be performed using a phosphoric acid electrolyte reaction.
Step 205: after the first protective layer is formed on the inner wall of the chamber by adopting a hard anodic oxidation mode, the inner wall of the chamber is cleaned and dried again. For example, the steps of water washing, compressed air blowing and hot air drying can be sequentially carried out for a plurality of times, so that impurities such as particles possibly generated in the prior process are fully removed.
Step 206: and vapor depositing the parylene coating to seal the hole of the first protective layer formed by the hard anodic oxidation, so as to form a uniform and compact second protective layer. Because a large number of holes exist in the material of the first protective layer formed by hard anodic oxidation, the material is subjected to deposition hole sealing by adopting the parylene coating, and the adhesive force between the parylene coating and the inner wall of the cavity can be improved.
Finally, step 207: the second protective layer formed by the parylene coating is further processed through oxygen plasma etching or high-frequency laser radiation, moderate etching is carried out on the second protective layer, the surface roughness of the parylene coating is optimized, the adhesion between layers which can be formed continuously in the subsequent process can be further improved, and the usability of the inner wall of the chamber is improved.
While, for purposes of simplicity of explanation, the methodologies are shown and described as a series of acts, it is to be understood and appreciated that the methodologies are not limited by the order of acts, as some acts may, in accordance with one or more embodiments, occur in different orders and/or concurrently with other acts from that shown and described herein or not shown and described herein, as would be understood and appreciated by those skilled in the art.
The previous description of the disclosure is provided to enable any person skilled in the art to make or use the disclosure. Various modifications to the disclosure will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other variations without departing from the spirit or scope of the disclosure. Thus, the disclosure is not intended to be limited to the examples and designs described herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A preparation method of a protective layer of the inner wall of a chamber comprises the following steps:
pretreating the inner wall of the chamber by sand blasting or HF pickling;
forming a first protection layer on the inner wall of the cavity by adopting a hard anodic oxidation mode; and
and depositing a parylene coating on the first protective layer to carry out hole sealing operation on the first protective layer, so as to form a second protective layer to finish the protective layer preparation work of the inner wall of the cavity.
2. The method for producing a protective layer according to claim 1, further comprising:
after the second protective layer is formed, oxygen plasma etching or high-frequency laser radiation is adopted to further optimize the second protective layer.
3. The method of claim 2, wherein the further optimizing the second protective layer by oxygen plasma etching or high frequency laser irradiation comprises:
the radiation intensity of the high-frequency laser radiation is changed to adjust the surface roughness of the second protective layer.
4. The method of manufacturing a protective layer according to claim 3, wherein the adjusting the surface roughness of the second protective layer comprises:
controlling the surface roughness Ra value of the second protective layer to be in the range of 0.025-12.5.
5. The method of producing a protective layer according to claim 1, wherein the forming a second protective layer comprises:
and controlling the formed second protective layer to be compact and nonporous, and ensuring that the thickness is uniform and is in the numerical range of 0.01-50 mu m.
6. The method for preparing a protective layer according to claim 1, wherein forming a first protective layer on the inner wall of the chamber by hard anodic oxidation comprises:
the hard anodic oxidation mode is realized by using phosphoric acid electrolyte for reaction.
7. The method for producing a protective layer according to claim 1, further comprising:
after the pretreatment of the inner wall of the chamber by sand blasting or HF pickling is performed, the inner wall of the chamber is cleaned by means of water washing or alkali washing.
8. The method for producing a protective layer according to claim 1, further comprising:
and after the first protective layer is formed on the inner wall of the chamber by adopting a hard anodic oxidation mode, cleaning and drying the inner wall of the chamber again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202310963147.XA CN116770386A (en) | 2023-07-31 | 2023-07-31 | Preparation method of protective layer on inner wall of chamber |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310963147.XA CN116770386A (en) | 2023-07-31 | 2023-07-31 | Preparation method of protective layer on inner wall of chamber |
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| CN116770386A true CN116770386A (en) | 2023-09-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118441240A (en) * | 2024-07-08 | 2024-08-06 | 上海派拉纶生物技术股份有限公司 | Micro array inner cavity device and protection method thereof |
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2023
- 2023-07-31 CN CN202310963147.XA patent/CN116770386A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118441240A (en) * | 2024-07-08 | 2024-08-06 | 上海派拉纶生物技术股份有限公司 | Micro array inner cavity device and protection method thereof |
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