CN111560599A - Process method for removing MPCVD (multi-layer chemical vapor deposition) cavity inner wall film - Google Patents
Process method for removing MPCVD (multi-layer chemical vapor deposition) cavity inner wall film Download PDFInfo
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- CN111560599A CN111560599A CN201911377222.4A CN201911377222A CN111560599A CN 111560599 A CN111560599 A CN 111560599A CN 201911377222 A CN201911377222 A CN 201911377222A CN 111560599 A CN111560599 A CN 111560599A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
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Abstract
The invention relates to a process method for removing a film on the inner wall of an MPCVD cavity, which comprises the following steps: sealing the MPCVD cavity and vacuumizing the MPCVD cavity; then all the air extraction valves are closed; gradually introducing etching gas into the MPCVD cavity; when the gas pressure reaches 0.6-1.5KPa, starting the microwave source to form plasma; then, etching gas is continuously and gradually introduced, the gas pressure and the microwave source power are increased, so that the temperature of the substrate table reaches a certain value and is maintained, and the corresponding cavity pressure is also unchanged within a certain value range; gradually increasing the power of the microwave source to a certain value, and maintaining the stable state for 25-40 min under the process condition; and finally, performing shutdown operation to finish the process of removing the film on the inner wall of the cavity and the impurity film on the surface of the substrate table. Impurity films on the inner wall of the MPCVD cavity, the surface of the substrate table, the quartz observation window and the like are thoroughly removed, so that impurities polluting diamond products are reduced, and the quality of synthesized products is improved.
Description
Technical Field
The invention relates to the technical field of production of diamond synthesized by an MPCVD (multi-phase chemical vapor deposition) method, in particular to a process method for removing a film on the inner wall of an MPCVD cavity.
Background
Diamond attracts attention because of its extremely excellent physicochemical properties. However, natural diamond reserves are limited, and thus various synthetic diamond methods such as a high temperature high pressure method (HPHT), a hot wire chemical vapor deposition method (HJCVD) have been developed. Wherein, the method for synthesizing diamond by Microwave plasma chemical vapor deposition (Microwave plasma chemical vapor deposition) can synthesize diamond with high quality and large area because no impurities are introduced.
The quality of diamond synthesized by MPCVD is related to many factors, including carbon source concentration, gas flow rate, temperature, substrate table height, microwave power, synthesis temperature, etc. However, in the process of synthesizing diamond by using the method, an impurity film is also deposited at a position with a temperature far lower than the growth temperature of diamond, such as the inner wall of a vacuum chamber, the surface of a substrate table, and the like, and the composition of the film has a great relationship with the temperature range of a specific position. In addition to the diamond phase, impurities such as diamond-like thin film and graphite may be generated, and such substances may adhere to the inner wall of the chamber or the surface of the substrate stage, and when reaching a certain thickness, warp or peel off from the inner wall or the surface of the substrate stage due to stress, and may scatter on the growth surface of the diamond, forming a contamination source, and affecting the growth quality of the final product.
Therefore, in order to avoid such a phenomenon, the inner wall of the vacuum chamber and the substrate stage must be cleaned and maintained regularly. The existing cleaning method is manual wiping, but the manual wiping efficiency is low, and because the inner space of the cavity is extremely limited, dead corners can not be completely removed frequently.
Disclosure of Invention
The invention provides a process method for removing a film on the inner wall of an MPCVD cavity, aiming at solving the problem of completely removing the film on the inner wall of the cavity and the surface of a substrate table, comprising the following steps:
s1, sealing the MPCVD cavity, and vacuumizing the MPCVD cavity;
s2, vacuumizing the MPCVD cavity to a certain vacuum degree, and then closing all extraction valves;
s3, gradually introducing etching gas into the MPCVD cavity with certain vacuum degree;
s4, when the gas pressure of the etching gas gradually introduced reaches 0.6-1.5KPa, starting a microwave source to form plasma;
s5, continuously and gradually introducing the etching gas, and increasing the gas pressure and the microwave source power to enable the temperature of the substrate table to reach a certain value;
s6, maintaining the temperature of the substrate table within a certain range of value and the corresponding cavity pressure unchanged within a certain range of value;
s7, under the condition of keeping the pressure of the cavity unchanged within a certain range of values, gradually increasing the power of the microwave source to a certain value, and maintaining the stable state for 25-40 minutes under the process condition;
and S8, finally, executing shutdown operation, and finishing the process of removing the film on the inner wall of the cavity and the impurity film on the surface of the substrate table.
Further, before the step S1, the diamond product is taken out of the MPCVD chamber, and the inner wall thereof is wiped.
Specifically, in the step S1, the vacuum process is performed, and the specific parameters of the vacuum process are related to the configured mechanical pump and molecular pump, and the vacuum process is generally performed for more than 5 minutes.
Specifically, the certain vacuum degree in the step S2 means that the vacuum degree is less than the gauge pressure value of 10-2pa。
Optionally, the etching gas in step S3 includes, but is not limited to, one of hydrogen, or a hydrogen/argon mixture, or a hydrogen/oxygen mixture, or a hydrogen/argon/oxygen mixture.
Preferably, the preferred gas pressure in step S4 reaches 0.9-1.2 KPa.
Preferably, the temperature of the substrate stage to a certain value in the step S5 is made to be any temperature value between 400 ℃ and 600 ℃, preferably any temperature value between 450 ℃ and 550 ℃.
Preferably, in step S6, when the temperature of the substrate stage reaches a certain value, the corresponding chamber pressure is also a certain value, and generally corresponds to a certain value between 15KP and 25KPa, and preferably a certain value between 18KP and 22 KP.
Specifically, in step S7, the microwave source power is increased to a certain value within the range of 4000-.
Preferably, in step S7, a steady state of 30-35 minutes is preferably maintained under the process conditions.
During the process of removing the film on the inner wall of the MPCVD cavity, an instrument for detecting the plasma species in real time, namely a plasma emission spectrometer (OES) can be added for observing the etching effect and progress in real time, and when the plasma species does not contain the C-related peak completely, the process of etching and removing the film is finished, and shutdown operation is executed.
The process method for removing the film on the inner wall of the MPCVD cavity has the main advantages that:
impurity films on the inner wall of the MPCVD cavity, the surface of the substrate table, the quartz observation window and the like are thoroughly removed, so that impurities polluting diamond products are reduced, and the quality of synthesized products is improved. The technological conditions for removing the film on the inner wall of the MPCVD cavity are adjusted and controlled according to specific conditions, and complete and thorough removal is ensured.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below.
Example 1:
a process method for removing the film on the inner wall of an MPCVD cavity comprises the following steps:
s1, sealing the MPCVD cavity, and vacuumizing the MPCVD cavity;
s2, vacuumizing the MPCVD cavity to a certain vacuum degree, wherein the vacuum degree is less than gauge pressure value 10-2pa, then closing all the air extraction valves;
s3, gradually introducing etching gas into the MPCVD cavity with certain vacuum degree;
s4, when the gas pressure of the etching gas gradually introduced reaches 0.6KPa, starting a microwave source to form plasma;
s5, continuously and gradually introducing the etching gas, and increasing the gas pressure and the microwave source power to enable the temperature of the substrate table to reach a certain value;
s6, maintaining the temperature of the substrate table within a certain range of value and the corresponding cavity pressure unchanged within a certain range of value; when the temperature of the substrate table reaches the set temperature, the temperature is stable by keeping the process parameters such as pressure, power and the like fixed;
s7, under the condition of keeping the pressure of the cavity unchanged within a certain range of values, gradually increasing the power of the microwave source to a certain value, and maintaining the stable state for 25 minutes under the process condition;
and S8, finally, executing shutdown operation, and finishing the process of removing the film on the inner wall of the cavity and the impurity film on the surface of the substrate table.
Prior to step S1, the diamond product is removed from the MPCVD chamber and its inner walls are wiped.
The specific parameters of the vacuum pumping process in step S1 are related to the configured mechanical pump and molecular pump, and the vacuum pumping process generally needs to be performed for more than 5 minutes.
In the step S2, the certain vacuum degree is required to be less than gauge pressure value 10-2pa。
In step S3, the etching gas is hydrogen.
The preferred gas pressure in step S4 reaches 0.9 KPa.
The step S5 is to make the temperature of the substrate table to a certain value be a temperature value of 400 ℃.
In step S6, when the temperature of the substrate stage reaches 400 ℃, the corresponding chamber pressure is constant, and generally corresponds to a constant value of 15 KP.
In step S7, the microwave source power is increased to a constant value of 4000 w.
Example 2:
a process method for removing the film on the inner wall of an MPCVD cavity comprises the following steps:
s1, sealing the MPCVD cavity, and vacuumizing the MPCVD cavity;
s2, vacuumizing the MPCVD cavity to a certain vacuum degree, wherein the vacuum degree is less than gauge pressure value 10-2pa, then closing all the air extraction valves;
s3, gradually introducing etching gas into the MPCVD cavity with certain vacuum degree;
s4, when the gas pressure of the etching gas gradually introduced reaches 0.6-1.5KPa, starting a microwave source to form plasma;
s5, continuously and gradually introducing the etching gas, and increasing the gas pressure and the microwave source power to enable the temperature of the substrate table to reach a certain value;
s6, maintaining the temperature of the substrate table within a certain range of value and the corresponding cavity pressure unchanged within a certain range of value;
s7, under the condition of keeping the pressure of the cavity unchanged within a certain range of values, gradually increasing the power of the microwave source to a certain value, and maintaining the stable state for 40 minutes under the process condition;
and S8, finally, executing shutdown operation, and finishing the process of removing the film on the inner wall of the cavity and the impurity film on the surface of the substrate table.
Prior to step S1, the diamond product is removed from the MPCVD chamber and its inner walls are wiped.
The specific parameters of the vacuum pumping process in step S1 are related to the configured mechanical pump and molecular pump, and the vacuum pumping process is generally performed for more than 5 minutes.
In the step S2, the certain vacuum degree is required to be less than gauge pressure value 10-2pa.。
In step S3, the etching gas is a hydrogen/argon gas mixture, and the volume ratio of the etching gas to the argon gas is 3:2 in this embodiment. Argon generally accounts for 10% -50% of the total volume.
The gas pressure in said step S4 reaches 1.2 KPa.
In step S5, the temperature of the substrate stage is set to 600 ℃.
In step S6, when the temperature of the substrate stage reaches a predetermined value, the corresponding chamber pressure is also constant at a predetermined value, corresponding to a predetermined value of 25 KPa.
In step S7, the microwave source power is increased to 6000 w.
Example 3:
a process method for removing the film on the inner wall of an MPCVD cavity comprises the following steps:
s1, sealing the MPCVD cavity, and vacuumizing the MPCVD cavity;
s2, vacuumizing the MPCVD cavity to a certain vacuum degree, wherein the vacuum degree is less than gauge pressure value 10-2pa, then closing all the air extraction valves;
s3, gradually introducing etching gas into the MPCVD cavity with certain vacuum degree;
s4, when the gas pressure of the etching gas gradually introduced reaches 1.0KPa, starting a microwave source to form plasma;
s5, continuously and gradually introducing the etching gas, and increasing the gas pressure and the microwave source power to enable the temperature of the substrate table to reach a certain value;
s6, maintaining the temperature of the substrate table within a certain range of value and the corresponding cavity pressure unchanged within a certain range of value;
s7, under the condition of keeping the pressure of the cavity unchanged within a certain range of values, gradually increasing the power of the microwave source to a certain value, and maintaining the stable state for 30 minutes under the process condition;
and S8, finally, executing shutdown operation, and finishing the process of removing the film on the inner wall of the cavity and the impurity film on the surface of the substrate table.
Prior to step S1, the diamond product is removed from the MPCVD chamber and its inner walls are wiped.
The specific parameters of the vacuum pumping process in step S1 are related to the configured mechanical pump and molecular pump, and the vacuum pumping process generally needs to be performed for more than 5 minutes.
In the step S2, the certain vacuum degree is required to be less than gauge pressure value 10-2pa.。
In step S3, the etching gas is a hydrogen/argon/oxygen mixture, and the volume ratio is 3:2:1 in this embodiment. Typically, hydrogen is present in an amount of more than 50% by volume.
The preferred gas pressure in step S4 is 1.0 KPa.
In step S5, the temperature of the substrate stage is set to a constant value of 500 ℃.
In step S6, when the temperature of the substrate stage reaches a certain value, the corresponding chamber pressure is also a certain value, and generally corresponds to a value of 20 KPa.
In step S7, the power of the microwave source is increased to a constant value of 5000 w.
Example 4:
a process method for removing the film on the inner wall of an MPCVD cavity comprises the following steps:
s1, sealing the MPCVD cavity, and vacuumizing the MPCVD cavity;
s2, vacuumizing the MPCVD cavity to a certain vacuum degree, wherein the vacuum degree is less than gauge pressure value 10-2pa, then closing all the air extraction valves;
s3, gradually introducing etching gas into the MPCVD cavity with certain vacuum degree;
s4, when the gas pressure of the etching gas gradually introduced reaches 1.1KPa, starting a microwave source to form plasma;
s5, continuously and gradually introducing the etching gas, and increasing the gas pressure and the microwave source power to enable the temperature of the substrate table to reach a certain value;
s6, maintaining the temperature of the substrate table within a certain range of value and the corresponding cavity pressure unchanged within a certain range of value;
s7, under the condition of keeping the pressure of the cavity unchanged within a certain range of values, gradually increasing the power of the microwave source to a certain value, and maintaining the stable state for 35 minutes under the process condition;
and S8, finally, executing shutdown operation, and finishing the process of removing the film on the inner wall of the cavity and the impurity film on the surface of the substrate table.
Prior to step S1, the diamond product is removed from the MPCVD chamber and its inner walls are wiped.
The specific parameters of the vacuum pumping process in step S1 are related to the configured mechanical pump and molecular pump, and the vacuum pumping process generally needs to be performed for more than 5 minutes.
In the step S2, the certain vacuum degree is required to be less than gauge pressure value 10-2pa。
Optionally, in step S3, the etching gas is a hydrogen/oxygen gas mixture, and the volume ratio is 4:2 in this embodiment. Oxygen is generally present in an amount of 10% to 50% by volume.
The preferred gas pressure in step S4 is 1.0 KPa.
In step S5, the temperature of the substrate stage is set to 550 ℃.
In step S6, when the temperature of the substrate stage reaches a certain value, the corresponding chamber pressure is also a certain value, and generally corresponds to a value of 22 KPa.
In step S7, the microwave source power is increased to a constant value of 5500 w.
Claims (10)
1. A process method for removing the film on the inner wall of an MPCVD cavity comprises the following steps:
s1, sealing the MPCVD cavity, and vacuumizing the MPCVD cavity;
s2, vacuumizing the MPCVD cavity to a certain vacuum degree, and then closing all extraction valves;
s3, gradually introducing etching gas into the MPCVD cavity with certain vacuum degree;
s4, when the gas pressure of the etching gas gradually introduced reaches 0.6-1.5KPa, starting a microwave source to form plasma;
s5, continuously and gradually introducing the etching gas, and increasing the gas pressure and the microwave source power to enable the temperature of the substrate table to reach a certain value;
s6, maintaining the temperature of the substrate table within a certain range of value and the corresponding cavity pressure unchanged within a certain range of value;
s7, under the condition of keeping the pressure of the cavity unchanged within a certain range of values, gradually increasing the power of the microwave source to a certain value, and maintaining the stable state for 25-40 minutes under the process condition;
and S8, finally, executing shutdown operation, and finishing the process of removing the film on the inner wall of the cavity and the impurity film on the surface of the substrate table.
2. The process of removing the film on the inner wall of the MPCVD chamber body according to claim 1, wherein before the step S1, the diamond product is taken out of the MPCVD chamber body and the inner wall thereof is wiped.
3. The process of claim 1 or 2, wherein the step S1 is performed by vacuum pumping, and the vacuum pumping is performed for more than 5 minutes according to the specific parameters related to the mechanical pump and the molecular pump.
4. The process for removing film on inner wall of MPCVD chamber of claim 1, wherein the certain vacuum degree in step S2 is a vacuum degree less than gauge pressure value of 10-2pa。
5. The process of claim 4, wherein the etching gas in step S3 includes but is not limited to hydrogen, or a mixture of hydrogen and argon, or a mixture of hydrogen and oxygen, or a mixture of hydrogen and argon and oxygen.
6. The process for removing the film on the inner wall of the MPCVD chamber body according to claim 5, wherein the preferred gas pressure in the step S4 is 0.9-1.2 KPa.
7. The process for removing the film on the inner wall of the MPCVD chamber body according to claim 1, wherein the temperature of the substrate table in step S5 is set to any temperature value between 400 ℃ and 600 ℃, preferably to any temperature value between 450 ℃ and 550 ℃.
8. The process of claim 1, wherein in step S6, when the temperature of the substrate stage reaches a certain value, the corresponding chamber pressure is constant, which generally corresponds to a certain value between 15KP and 25KPa, preferably a certain value between 18KP and 22 KP.
9. The process for removing the thin film on the inner wall of the MPCVD chamber as recited in claim 1, wherein in the step S7, the microwave source power is increased to a value within the range of 4000-6000 w.
10. The process for removing the film on the inner wall of the MPCVD chamber of claim 9, wherein in step S7, the process condition is preferably maintained at a steady state for 30-35 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114496703A (en) * | 2021-11-04 | 2022-05-13 | 上海稷以科技有限公司 | Method for realizing stable etching rate in large-scale mass production |
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| US6176936B1 (en) * | 1997-07-22 | 2001-01-23 | Nec Corporation | In-situ chamber cleaning method of CVD apparatus |
| CN101118378A (en) * | 2007-08-22 | 2008-02-06 | 武汉工程大学 | Preparation method of diamond surface graphics |
| CN106967961A (en) * | 2017-04-14 | 2017-07-21 | 王宏兴 | A kind of method of removal CVD reaction cavity inwall deposition films |
| CN109537052A (en) * | 2018-11-27 | 2019-03-29 | 西安碳星半导体科技有限公司 | A kind of pretreated method of CVD single crystal diamond film |
| CN110055514A (en) * | 2019-06-11 | 2019-07-26 | 厦门乾照光电股份有限公司 | Vapor deposition apparatus and its control method, cavity clean method |
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2019
- 2019-12-27 CN CN201911377222.4A patent/CN111560599A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6176936B1 (en) * | 1997-07-22 | 2001-01-23 | Nec Corporation | In-situ chamber cleaning method of CVD apparatus |
| CN101118378A (en) * | 2007-08-22 | 2008-02-06 | 武汉工程大学 | Preparation method of diamond surface graphics |
| CN106967961A (en) * | 2017-04-14 | 2017-07-21 | 王宏兴 | A kind of method of removal CVD reaction cavity inwall deposition films |
| CN109537052A (en) * | 2018-11-27 | 2019-03-29 | 西安碳星半导体科技有限公司 | A kind of pretreated method of CVD single crystal diamond film |
| CN110055514A (en) * | 2019-06-11 | 2019-07-26 | 厦门乾照光电股份有限公司 | Vapor deposition apparatus and its control method, cavity clean method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114496703A (en) * | 2021-11-04 | 2022-05-13 | 上海稷以科技有限公司 | Method for realizing stable etching rate in large-scale mass production |
| CN114496703B (en) * | 2021-11-04 | 2023-10-10 | 上海稷以科技有限公司 | Method for realizing stable etching rate in large-scale mass production |
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