CN115652283A - MOCVD cavity covering part cleaning method - Google Patents
MOCVD cavity covering part cleaning method Download PDFInfo
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- CN115652283A CN115652283A CN202211670564.7A CN202211670564A CN115652283A CN 115652283 A CN115652283 A CN 115652283A CN 202211670564 A CN202211670564 A CN 202211670564A CN 115652283 A CN115652283 A CN 115652283A
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- 238000004140 cleaning Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 title abstract 2
- 239000007789 gas Substances 0.000 claims abstract description 115
- 239000012159 carrier gas Substances 0.000 claims abstract description 69
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 22
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000460 chlorine Substances 0.000 claims abstract description 18
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- NBRKLOOSMBRFMH-UHFFFAOYSA-N tert-butyl chloride Chemical compound CC(C)(C)Cl NBRKLOOSMBRFMH-UHFFFAOYSA-N 0.000 claims description 11
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical class CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 4
- RNQKDQAVIXDKAG-UHFFFAOYSA-N aluminum gallium Chemical compound [Al].[Ga] RNQKDQAVIXDKAG-UHFFFAOYSA-N 0.000 description 14
- 239000011248 coating agent Substances 0.000 description 13
- 238000000576 coating method Methods 0.000 description 13
- 150000002259 gallium compounds Chemical class 0.000 description 13
- 229910052782 aluminium Inorganic materials 0.000 description 11
- -1 aluminum gallium metal compounds Chemical class 0.000 description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 10
- 229910010271 silicon carbide Inorganic materials 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000005530 etching Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 229910002601 GaN Inorganic materials 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000000407 epitaxy Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
A method for cleaning an MOCVD cavity covering part relates to the technical field of semiconductors and comprises the following steps: heating the cavity to a first preset temperature, and introducing a first mixed gas of chlorine and a first carrier gas into the cavity to clean the covering part for a first preset time; heating the cavity to a second preset temperature, and introducing a second mixed gas of ammonia gas and first carrier gas or a third mixed gas of ammonia gas and second carrier gas into the cavity to clean the covering part for a second preset time; heating the cavity to a third preset temperature, and introducing a fourth mixed gas of hydrogen chloride and a first carrier gas, a fifth mixed gas of hydrogen chloride and a second carrier gas, a sixth mixed gas of chlorinated tert-butane and the first carrier gas or a seventh mixed gas of chlorinated tert-butane and the second carrier gas into the cavity to clean the covering piece for a third preset time; and heating the cavity to a fourth preset temperature, and introducing hydrogen into the cavity to clean the covering part for a fourth preset time. The cleaning method can improve the stability of the process and the service life of the covering element.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a cleaning method for an MOCVD (metal organic chemical vapor deposition) cavity covering piece.
Background
Metal Organic Chemical Vapor Deposition (MOCVD) equipment is widely applied to epitaxial preparation of second-generation and third-generation semiconductor materials, however, after each epitaxial formula growth is completed, a layer of chemical reactant is attached to a covering part (usually a graphite part) in a cavity, which affects the growth of the next epitaxial material and the stability of the process, and particularly affects the third-generation semiconductor based on gallium nitride epitaxy of a silicon substrate greatly, because the attachment on the covering part corrodes the silicon substrate, the subsequent epitaxial process fails.
The existing cleaning method of the cavity covering part comprises the following steps: the method comprises the steps of detaching a covering part, moving the covering part out of a reaction chamber, placing the covering part in a high-temperature baking furnace, blowing the covering part by using hydrogen or a hydrogen-nitrogen mixture gas at high temperature and low pressure, blowing the attachments on the covering part clean, and then placing the covering part in an MOCVD reaction chamber for the next epitaxial formula growth; and secondly, the covering part is not replaced, chlorine is introduced into the cavity after the cavity is heated to a certain temperature to react with the aluminum, the gallium and the aluminum-gallium compound, and the epitaxial formula growth is carried out after the attachments on the surface of the covering part are removed.
The prior MOCVD cavity covering part cleaning technology has the following defects: in the first method, the production time is reduced and the productivity is reduced by replacing the covering part, and the process repeatability is influenced by frequently replacing the covering part; in the second method, chlorine is introduced to remove the aluminum, gallium and aluminum gallium metal compounds on the cavity covering piece, but the cleaning effect is deteriorated when the attachments of the active carbon-doped epitaxial layer are met; in addition, due to the strong corrosivity of chlorine, when the attachments are cleaned up quickly, the chlorine can corrode the coating (usually silicon carbide coating) on the covering piece, so that the service life of the covering piece is shortened, and the production cost is increased.
Disclosure of Invention
The invention aims to provide a cleaning method of an MOCVD cavity covering part, which does not need to disassemble the covering part, can avoid reducing the productivity and improve the process stability, and meanwhile, has lower corrosivity on the covering part, can prolong the service life of the covering part, thereby reducing the production cost.
The embodiment of the invention is realized by the following steps:
the embodiment of the invention provides a method for cleaning a MOCVD (metal organic chemical vapor deposition) cavity covering piece, which comprises the following steps of: heating the cavity to a first preset temperature, and introducing a first mixed gas of chlorine and a first carrier gas into the cavity to clean the covering part for a first preset time; heating the cavity to a second preset temperature, and introducing a second mixed gas of ammonia gas and first carrier gas or a third mixed gas of ammonia gas and second carrier gas into the cavity to clean the covering element for a second preset time; heating the cavity to a third preset temperature, and introducing a fourth mixed gas of hydrogen chloride and a first carrier gas, a fifth mixed gas of hydrogen chloride and a second carrier gas, a sixth mixed gas of tert-butyl chloride and the first carrier gas or a seventh mixed gas of tert-butyl chloride and the second carrier gas into the cavity to clean the covering piece for a third preset time; and heating the cavity to a fourth preset temperature, and introducing hydrogen into the cavity to clean the covering element for a fourth preset time.
As a practical way, the heating the cavity to the first preset temperature and the heating the cavity to the second preset temperature are repeatedly performed at least twice.
As a practical manner, the heating the cavity to the second preset temperature and the heating the cavity to the third preset temperature are repeatedly performed at least twice.
As an implementation mode, when a cavity is heated to a first preset temperature, the air pressure of the cavity is 70mbar to 150mbar, the first preset temperature is 800 ℃ to 900 ℃, the flow rate of chlorine of the first mixed gas is 20L/min to 30L/min, and the flow rate of the first carrier gas of the first mixed gas is 10L/min to 30L/min.
In an embodiment, the concentration of the chlorine gas in the first mixed gas is between 3% and 10%, and the concentration of the first carrier gas in the first mixed gas is 100%.
As an implementation mode, when the cavity is heated to a second preset temperature, the air pressure of the cavity is 50mbar to 100mbar, the second preset temperature is 1100 to 1160 ℃, the flow rate of ammonia of the second mixed gas is 15L/min to 25L/min, and the flow rate of the second carrier gas of the second mixed gas is 15L/min to 25L/min.
As an implementation mode, when the cavity is heated to a third preset temperature, the air pressure of the cavity is 50mbar to 100mbar, the third preset temperature is 600 to 1000 ℃, the flow of hydrogen chloride of the fourth mixed gas is 5L/min to 10L/min, and the flow of the second carrier gas of the fourth mixed gas is 20L/min to 50L/min.
As an implementation mode, when the cavity is heated to a fourth preset temperature, the air pressure of the cavity is 50mbar to 100mbar, the fourth preset temperature is more than 1100 ℃, and the flow rate of the hydrogen is 80L/min to 150L/min.
In one possible implementation, the first carrier gas is nitrogen and the second carrier gas is hydrogen.
The embodiment of the invention has the beneficial effects that:
the cleaning method comprises the steps of heating a cavity to a first preset temperature, and introducing a first mixed gas of chlorine and a first carrier gas into the cavity to clean a covering piece for a first preset time period so as to remove an aluminum compound, a gallium compound and an aluminum gallium compound attached to the covering piece; heating the cavity to a second preset temperature, and introducing a second mixed gas of ammonia gas and first carrier gas or a third mixed gas of ammonia gas and second carrier gas into the cavity to clean the covering piece for a second preset time so as to remove carbon-containing attachments on the covering piece; the cavity is heated to a third preset temperature, and a fourth mixed gas of hydrogen chloride and a first carrier gas, a fifth mixed gas of hydrogen chloride and a second carrier gas, a sixth mixed gas of tert-butyl chloride and the first carrier gas or a seventh mixed gas of tert-butyl chloride and the second carrier gas are introduced into the cavity to clean the covering piece for a third preset time, so that aluminum compounds, gallium compounds and aluminum gallium compounds attached to the covering piece can be removed, and corrosion to a silicon carbide coating on the covering piece can be reduced; the cavity is heated to a fourth preset temperature, and hydrogen is introduced into the cavity to clean the covering piece for a fourth preset time so as to sweep the attachments on the covering piece completely, and the covering piece is thoroughly cleaned in the last step, so that preparation is made for the next epitaxial formula growth. The cleaning method provided by the application is an in-situ cleaning method, namely the movable covering part does not need to be detached, the covering part can be cleaned in an MOCVD cavity, so that the yield can be prevented from being reduced, the process stability is improved, and meanwhile, the fourth mixed gas (fifth mixed gas, sixth mixed gas or seventh mixed gas) is low in corrosivity to a silicon carbide coating on the covering part, so that the service life of the covering part can be prolonged, and the production cost is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is one of the flow charts of the MOCVD chamber cover cleaning method according to the embodiment of the present invention;
fig. 2 is a second flowchart of a cleaning method for an MOCVD chamber cover according to an embodiment of the present invention;
fig. 3 is a third flowchart of the MOCVD chamber cover cleaning method according to the embodiment of the present invention.
Detailed Description
The embodiments set forth below represent the necessary information to enable those skilled in the art to practice the embodiments and illustrate the best mode of practicing the embodiments. Upon reading the following description in light of the accompanying drawing figures, those skilled in the art will understand the concepts of the disclosure and will recognize applications of these concepts not particularly addressed herein. It should be understood that these concepts and applications fall within the scope of the disclosure and the accompanying claims.
It will be understood that, although the terms first, second, etc. may be used herein to describe various elements, these elements should not be limited by these terms. These terms are only used to distinguish one element from another. For example, a first element could be termed a second element, and, similarly, a second element could be termed a first element, without departing from the scope of the present disclosure. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
It will be understood that when an element such as a layer, region or substrate is referred to as being "on" or "extending" onto "another element, it can be directly on or extend directly onto the other element or intervening elements may also be present. In contrast, when an element is referred to as being "directly on" or extending "directly onto" another element, there are no intervening elements present. Also, it will be understood that when an element such as a layer, region or substrate is referred to as being "on" or "extending over" another element, it can be directly on or extend directly over the other element or intervening elements may also be present. In contrast, when an element is referred to as being "directly on" or extending "directly over" another element, there are no intervening elements present. It will also be understood that when an element is referred to as being "connected" or "coupled" to another element, it can be directly connected or coupled to the other element or intervening elements may be present. In contrast, when an element is referred to as being "directly connected" or "directly coupled" to another element, there are no intervening elements present.
Relative terms such as "below …" or "above …" or "upper" or "lower" or "horizontal" or "vertical" may be used herein to describe one element, layer or region's relationship to another element, layer or region, as illustrated in the figures.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used herein, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. It will be further understood that terms used herein should be interpreted as having a meaning that is consistent with their meaning in the context of this specification and the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Referring to fig. 1 to 3, the present application provides a method for cleaning a covering part of an MOCVD chamber, which is used between two epitaxial growth processes to clean the covering part, and after the previous epitaxial growth is finished, the covering part is cleaned by the cleaning method provided by the present application, so that the next epitaxial growth can be started. The cleaning method provided by the application can avoid reducing the productivity and improve the process stability because the covering part is not required to be disassembled, and can prolong the service life of the covering part because the corrosivity to the covering part is lower, thereby reducing the production cost.
Specifically, as shown in fig. 1, the method for cleaning the MOCVD chamber cover comprises the following steps:
s100, heating the cavity to a first preset temperature, and introducing a first mixed gas of chlorine and a first carrier gas into the cavity to clean the covering part for a first preset time;
in the first mixed gas, chlorine gas is a cleaning gas having high corrosiveness and capable of removing aluminum compounds, gallium compounds, and aluminum gallium compounds adhering to the coating material, and the first carrier gas is an auxiliary gas and is a gas that does not react with chlorine gas. Specifically, the chlorine gas reacts with the aluminum compound, the gallium compound and the aluminum gallium compound attached to the covering part, and chloride and nitrogen gas can be generated and discharged out of the cavity, so that the purpose of cleaning the aluminum compound, the gallium compound and the aluminum gallium compound attached to the covering part is achieved. The step can adjust the first preset time according to the growth thickness of the epitaxial layer, so that most of the thickness of the attachments on the cover is etched (for example, 80% -90%). However, when the first mixed gas encounters the active carbon-doped gallium nitride epitaxial layer, the cleaning effect of chlorine on carbon-containing attachments on the cover member is poor, and if the active carbon-doped layer is thick, the cleaning effect of chlorine on aluminum compounds, gallium compounds and aluminum-gallium compounds attached on the cover member is poor due to the attachment of carbon doped impurities, so that the conditions for repeated growth of each epitaxy are slightly changed, thereby affecting the performance of the device.
S200, heating the cavity to a second preset temperature, and introducing a second mixed gas of ammonia and first carrier gas or a third mixed gas of ammonia and second carrier gas into the cavity to clean the covering part for a second preset time;
it should be noted that, in order to solve the above problem, the cleaning method provided by the present application further cleans the covering member by introducing a second mixed gas of ammonia gas and the first carrier gas or a third mixed gas of ammonia gas and the second carrier gas into the chamber. In the second mixed gas and the third mixed gas, ammonia gas is used as a cleaning gas and has certain corrosiveness, carbon-containing attachments on the covering piece can be removed, and the first carrier gas and the second carrier gas are used as auxiliary gases and are gases which cannot react with the ammonia gas. Specifically, at a certain temperature, the ammonia gas can react with the carbon-containing attachments on the covering part to generate hydrogen cyanide gas and hydrogen gas which are discharged out of the cavity, so that the purpose of cleaning the carbon-containing attachments on the covering part is achieved. Then, the aluminum compound, the gallium compound, and the aluminum-gallium compound adhering to the cover member are cleaned with chlorine gas, and the cleaning effect is improved.
S300, heating the cavity to a third preset temperature, and introducing a fourth mixed gas of hydrogen chloride and a first carrier gas, a fifth mixed gas of hydrogen chloride and a second carrier gas, a sixth mixed gas of tert-butyl chloride and the first carrier gas or a seventh mixed gas of tert-butyl chloride and the second carrier gas into the cavity to clean the covering piece for a third preset time;
it should be noted that, because chlorine has high corrosivity, it is difficult to ensure that only the deposit on the cover is etched by chlorine in the actual cleaning process, but instead, the coating (e.g., silicon carbide coating) on the cover is easily corroded, so that the service life of the cover is reduced. For this purpose, after the thickness of the attachments on the covering part is mostly etched by chlorine gas, the cleaning method provided by the application also cleans the covering part by introducing a fourth mixed gas of hydrogen chloride and a first carrier gas, a fifth mixed gas of hydrogen chloride and a second carrier gas, a sixth mixed gas of tert-butyl chloride and the first carrier gas or a seventh mixed gas of tert-butyl chloride and the second carrier gas into the cavity. In the fourth mixed gas and the fifth mixed gas, hydrogen chloride is used as a cleaning gas, aluminum compounds, gallium compounds and aluminum gallium compounds attached to the covering part can be removed, but the corrosion to a silicon carbide coating on the covering part is low, so that the service life of the covering part can be prolonged, and the production cost can be reduced, and the first carrier gas and the second carrier gas are used as auxiliary gases and are gases which do not react with hydrogen chloride. Since the chlorinated tert-butane is heated to a certain temperature and then decomposes the hydrogen chloride gas, the chlorinated tert-butane can be used in the sixth mixed gas and the seventh mixed gas to replace the hydrogen chloride gas, so that not only can the aluminum compound, the gallium compound and the aluminum gallium compound attached to the covering piece be removed, but also the corrosion to the silicon carbide coating on the covering piece can be reduced, and the first carrier gas and the second carrier gas are used as auxiliary gases and are gases which do not react with the chlorinated tert-butane and the hydrogen chloride.
S400, heating the cavity to a fourth preset temperature, and introducing hydrogen into the cavity to clean the covering part for a fourth preset time.
It should be noted that in the cleaning method provided by the application, the covering part is purged by introducing hydrogen into the cavity to purge the attachments on the covering part, and the covering part is thoroughly cleaned in the last step, so that preparation is made for the next epitaxial formula growth.
According to the cleaning method provided by the application, the cavity is heated, and the first mixed gas, the second mixed gas (or the third mixed gas), the fourth mixed gas (the fifth mixed gas, the sixth mixed gas or the seventh mixed gas) and the hydrogen are sequentially introduced into the cavity, so that the aluminum compound, the gallium compound and the aluminum gallium compound which are attached to the covering part, the carbon-containing attachment on the covering part, the aluminum compound, the gallium compound and the aluminum gallium compound which are attached to the covering part and the attachment on the covering part are respectively cleaned, and therefore the cleaning effect is improved. Moreover, the cleaning method provided by the application is an in-situ cleaning method, namely the movable covering part is not required to be disassembled, the covering part can be cleaned in an MOCVD cavity, so that the productivity can be prevented from being reduced, the process stability is improved, and meanwhile, the fourth mixed gas (the fifth mixed gas, the sixth mixed gas or the seventh mixed gas) is low in corrosivity on the silicon carbide coating on the covering part, so that the service life of the covering part can be prolonged, and the production cost is reduced.
As shown in fig. 2, as an implementable manner, the steps of S100, heating the chamber to the first preset temperature and S200, and heating the chamber to the second preset temperature are repeatedly performed at least twice (i.e., m is greater than or equal to 2). In other words, after the first time S100, the heating of the chamber to the first preset temperature and S200, and the heating of the chamber to the second preset temperature are finished, the step S100, the step S200, the step S300, and the step S200 are performed at least once again, and the step S of heating the chamber to the third preset temperature are performed, so that not only can the purpose of completely cleaning the attachments on the covering member be achieved, but also the corrosion damage to the silicon carbide coating on the covering member can be reduced.
As a practical manner, the steps of S200, heating the chamber to the second preset temperature and S300, and heating the chamber to the third preset temperature are repeatedly performed at least twice (i.e., n is greater than or equal to 2). In other words, after the first time S200, the heating of the chamber to the second preset temperature and S300, and the heating of the chamber to the third preset temperature are finished, the step S200, the step S300, the step S400, and the step S400 are performed at least once again, so that not only can the purpose of completely cleaning the attachments on the covering member be achieved, but also the corrosion damage to the silicon carbide coating on the covering member can be reduced.
As an implementation manner, when the cavity is heated to the first predetermined temperature, the air pressure of the cavity is between 70mbar and 150mbar, such as 70mbar, 90mbar, 100mbar, 120mbar, or 150mbar, and the like, the first predetermined temperature is between 800 ℃ and 900 ℃, such as 800 ℃, 820 ℃, 850 ℃, 870 ℃, or 900 ℃, and the like, it is noted that the first predetermined temperature may not exceed 900 ℃ so as to avoid aggravating corrosion of the silicon carbide coating on the covering part, the flow rate of the chlorine gas of the first mixed gas is between 20L/min and 30L/min, such as 20L/min, 22L/min, 25L/min, 28L/min, or 30L/min, and the flow rate of the first carrier gas of the first mixed gas is between 10L/min and 30L/min, such as 10L/min, 15L/min, 20L/min, 25L/min, or 30L/min, and the like, so as to improve the etching efficiency of the aluminum compound, the gallium compound, and the aluminum gallium compound adhered on the covering part. The gas pressure of the chamber, the first preset temperature, the flow rate of the chlorine in the first mixed gas, and the flow rate of the first carrier gas in the first mixed gas, which are described above, should be reasonably selected and designed by those skilled in the art according to practical situations, and are not limited in particular.
As an embodiment, the concentration of the chlorine gas in the first mixed gas is between 3% and 10%, for example, 3%, 5%, 7%, 9%, or 10%, and the concentration of the first carrier gas in the first mixed gas is 100%. The concentration of chlorine in the first mixed gas is not particularly limited, and those skilled in the art can reasonably select and design the concentration according to practical situations.
As an implementation manner, when the cavity is heated to the second predetermined temperature, the air pressure of the cavity is 50mbar to 100mbar, such as 50mbar, 60mbar, 75mbar, 90mbar or 100mbar, etc., the second predetermined temperature is 1100 to 1160 ℃, such as 1100 ℃, 1110 ℃, 1130 ℃, 1150 ℃ or 1160 ℃, etc., the flow rate of the ammonia gas of the second mixed gas is 15L/min to 25L/min, such as 15L/min, 17L/min, 20L/min, 22L/min or 25L/min, etc., and the flow rate of the second carrier gas of the second mixed gas is 15L/min to 25L/min, such as 15L/min, 17L/min, 20L/min, 22L/min or 25L/min, etc., so as to improve the etching efficiency of the carbon-containing attachments on the covering part. The pressure of the chamber, the second preset temperature, the flow rate of the ammonia gas of the second mixed gas, and the flow rate of the second carrier gas of the second mixed gas, which are mentioned above, should be reasonably selected and designed by those skilled in the art according to practical situations, and are not limited herein.
As an implementation manner, when the cavity is heated to a third predetermined temperature, the air pressure of the cavity is 50mbar to 100mbar, such as 50mbar, 60mbar, 75mbar, 90mbar or 100mbar, the third predetermined temperature is 600 to 1000 ℃, such as 600 ℃, 700 ℃, 800 ℃, 900 ℃ or 1000 ℃, the flow rate of the hydrogen chloride of the fourth mixed gas is 5L/min to 10L/min, such as 5L/min, 6L/min, 7L/min, 9L/min or 10L/min, and the flow rate of the second carrier gas of the fourth mixed gas is 20L/min to 50L/min, such as 20L/min, 25L/min, 30L/min, 40L/min or 50L/min, so as to improve the accuracy of etching the aluminum compound, the gallium compound and the aluminum gallium compound attached to the covering part. The gas pressure of the chamber, the third preset temperature, the flow rate of the hydrogen chloride of the fourth mixed gas, and the flow rate of the second carrier gas of the fourth mixed gas, which are described above, should be reasonably selected and designed by those skilled in the art according to actual situations, and are not limited herein.
As an implementation manner, when the cavity is heated to the fourth preset temperature, the air pressure of the cavity is 50mbar to 100mbar, such as 50mbar, 60mbar, 75mbar, 90mbar or 100mbar, etc., the fourth preset temperature is over 1100 ℃, such as 1100 ℃, 1200 ℃, 1300 ℃, 1500 ℃ or 1600 ℃, etc., the flow rate of the hydrogen is between 80L/min to 150L/min, such as 80L/min, 100L/min, 120L/min, 130L/min or 150L/min, etc., so as to purge the attachments on the covering element through a large amount of high-temperature hydrogen, thereby further thoroughly cleaning the attachments on the covering element and preventing the attachments from remaining on the covering element. The gas pressure and the flow rate of the hydrogen gas in the chamber are appropriately selected and designed by those skilled in the art according to practical situations, and are not particularly limited herein.
As one practical way, the first carrier gas is nitrogen and the second carrier gas is hydrogen. When neither nitrogen nor hydrogen reacts with the purge gas (including ammonia, hydrogen chloride and chlorot-butane), the load of the pump of the apparatus is inevitably increased as compared with the case of nitrogen having a large specific gravity, and hydrogen may be preferably used as the auxiliary gas.
The above description is only an alternative embodiment of the present invention and is not intended to limit the present invention, and various modifications and variations of the present invention may occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (9)
1. A cleaning method for an MOCVD (metal organic chemical vapor deposition) cavity covering part is characterized by comprising the following steps:
heating the cavity to a first preset temperature, and introducing a first mixed gas of chlorine and a first carrier gas into the cavity to clean the covering part for a first preset time;
heating the cavity to a second preset temperature, and introducing a second mixed gas of ammonia and a first carrier gas or a third mixed gas of ammonia and the second carrier gas into the cavity to clean the covering piece for a second preset time;
heating the cavity to a third preset temperature, and introducing a fourth mixed gas of hydrogen chloride and a first carrier gas, a fifth mixed gas of hydrogen chloride and a second carrier gas, a sixth mixed gas of tert-butyl chloride and the first carrier gas or a seventh mixed gas of tert-butyl chloride and the second carrier gas into the cavity to clean the covering piece for a third preset time;
and heating the cavity to a fourth preset temperature, and introducing hydrogen into the cavity to clean the covering piece for a fourth preset time.
2. The MOCVD chamber cover cleaning method according to claim 1, wherein the heating of the chamber to the first preset temperature and the heating of the chamber to the second preset temperature are repeatedly performed at least twice.
3. The MOCVD chamber cover cleaning method according to claim 1, wherein the heating the chamber to the second preset temperature and the heating the chamber to the third preset temperature are repeatedly performed at least twice.
4. The cleaning method for the MOCVD cavity covering part, according to claim 1, is characterized in that when the cavity is heated to a first preset temperature, the air pressure of the cavity is 70mbar to 150mbar, the first preset temperature is 800 ℃ to 900 ℃, the flow rate of chlorine of the first mixed gas is 20L/min to 30L/min, and the flow rate of the first carrier gas of the first mixed gas is 10L/min to 30L/min.
5. The MOCVD chamber cover cleaning method according to claim 1, wherein the concentration of chlorine in the first mixed gas is between 3% and 10%, and the concentration of the first carrier gas in the first mixed gas is 100%.
6. The cleaning method for the MOCVD cavity covering part, according to claim 1, is characterized in that when the cavity is heated to a second preset temperature, the air pressure of the cavity is 50mbar to 100mbar, the second preset temperature is 1100 ℃ to 1160 ℃, the flow rate of ammonia gas of the second mixed gas is 15L/min to 25L/min, and the flow rate of a second carrier gas of the second mixed gas is 15L/min to 25L/min.
7. The cleaning method for the MOCVD cavity covering part, according to claim 1, is characterized in that when the cavity is heated to a third preset temperature, the air pressure of the cavity is 50mbar to 100mbar, the third preset temperature is 600 ℃ to 1000 ℃, the flow rate of hydrogen chloride of the fourth mixed gas is 5L/min to 10L/min, and the flow rate of a second carrier gas of the fourth mixed gas is 20L/min to 50L/min.
8. The cleaning method for the MOCVD cavity covering part, according to claim 1, is characterized in that when the cavity is heated to a fourth preset temperature, the air pressure of the cavity is 50mbar to 100mbar, the fourth preset temperature is more than 1100 ℃, and the flow rate of the hydrogen is 80L/min to 150L/min.
9. The MOCVD chamber cover cleaning method according to claim 1, wherein the first carrier gas is nitrogen and the second carrier gas is hydrogen.
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Application publication date: 20230131 |