CN117737695A - Cleaning method - Google Patents
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- CN117737695A CN117737695A CN202311764326.7A CN202311764326A CN117737695A CN 117737695 A CN117737695 A CN 117737695A CN 202311764326 A CN202311764326 A CN 202311764326A CN 117737695 A CN117737695 A CN 117737695A
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- 238000004140 cleaning Methods 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 53
- 239000004642 Polyimide Substances 0.000 claims abstract description 34
- 229920001721 polyimide Polymers 0.000 claims abstract description 34
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 26
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 238000000197 pyrolysis Methods 0.000 claims abstract description 14
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 9
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims abstract description 9
- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 9
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 23
- 229920001046 Nanocellulose Polymers 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 21
- 238000000137 annealing Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- 238000004807 desolvation Methods 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- AJFDBNQQDYLMJN-UHFFFAOYSA-N n,n-diethylacetamide Chemical compound CCN(CC)C(C)=O AJFDBNQQDYLMJN-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000000151 deposition Methods 0.000 description 11
- 230000008021 deposition Effects 0.000 description 11
- 238000005229 chemical vapour deposition Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 125000001153 fluoro group Chemical group F* 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Abstract
The invention relates to the field of silicon carbide cleaning, and provides a cleaning method, which comprises the steps of cleaning a silicon carbide-containing deposit on the surface of a substrate by using a cleaning gas; the substrate comprises a pyrolytic carbon coating on the surface of a base; the pyrolytic carbon coating is obtained by pyrolysis of polyimide and nano microcrystalline cellulose; the cleaning gas is chlorine trifluoride. The method can enable the silicon carbide film or particles to fall off from the surface of pyrolytic carbon, so that the cleaning of the CVD reactor is realized, meanwhile, the corrosion of chlorine trifluoride to the reactor and a substrate can be reduced, and the service life of the reactor is prolonged.
Description
Technical Field
The invention relates to the field of silicon carbide cleaning, in particular to a cleaning method.
Background
Silicon carbide is an important ceramic material and is grown epitaxially by Chemical Vapor Deposition (CVD). However, during epitaxial growth, because of long-term reaction in the CVD deposition furnace, siC coatings of certain thickness are deposited on the walls, susceptor surfaces and ports of the reaction chamber, too thick coatings can clog the ports, and these films often emit small particles that contaminate the deposited sample, resulting in lattice defects.
To remove deposited silicon carbide, the furnace is maintainedCleaning conditions for deposition, such as chlorine trifluoride (ClF) 3 ) The CVD reactor cleaning process is performed using a gas or the like as a cleaning gas. However, since chlorine trifluoride is likely to react with graphite, silicon carbide can be removed using chlorine trifluoride when cleaning with chlorine trifluoride, but at the same time, since graphite has high corrosion reactivity, damage to a reaction vessel, a susceptor, and the like is likely to occur.
Therefore, there is a need to develop a method for cleaning silicon carbide more safely, so as to reduce the damage of the reactor and prolong the service life of the reactor.
Disclosure of Invention
The present invention has been made to overcome the above-mentioned problems occurring in the prior art, and an object of the present invention is to provide a cleaning method by which the purpose of cleaning silicon carbide can be more safely achieved.
In order to achieve the above object, the present invention provides a cleaning method comprising: cleaning a silicon carbide-containing deposit located on a surface of a substrate using a cleaning gas; the substrate comprises a pyrolytic carbon coating on the surface of a base;
the pyrolytic carbon coating is obtained by pyrolysis of polyimide and nano microcrystalline cellulose;
the cleaning gas is chlorine trifluoride.
The technical scheme adopted by the invention has the following beneficial effects:
(1) The invention uses chlorine trifluoride (ClF) 3 ) The PI/NCC pyrolytic carbon film is used as cleaning gas and is used as a coating material on the surface of the carbon sensor to carry out a CVD reactor cleaning process, the silicon carbide film or particles can fall off from the surface of the pyrolytic carbon film, the surface of the pyrolytic carbon film is not easy to damage and doped with impurities, fluorine atoms are diffused outwards through annealing in a nitrogen environment containing a trace amount of oxygen, the damage of the CVD reactor can be further reduced, and meanwhile, the cleaning of the CVD reactor is ensured.
(2) The method provided by the invention can also prolong the service life of the reactor.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein. Herein, unless otherwise specified, data ranges all include endpoints.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
Unless defined otherwise, all scientific and technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention relates.
The invention provides a cleaning method, which comprises the following steps: cleaning a silicon carbide-containing deposit located on a surface of a substrate using a cleaning gas; the substrate comprises a pyrolytic carbon coating on the surface of a base;
the pyrolytic carbon coating is obtained by pyrolysis of Polyimide (PI) and nanocrystalline cellulose (NCC);
the cleaning gas is chlorine trifluoride.
In the present invention, the base material means an inner wall of an apparatus for manufacturing, for example, a silicon carbide single crystal (for example, in the form of a silicon carbide epitaxial film) or an accessory thereof (for example, a susceptor for setting a semiconductor wafer).
In the present invention, the substrate may be a material capable of withstanding the formation temperature of the silicon carbide single crystal, such as a carbon material (e.g., graphite), silicon carbide, or a carbon/silicon carbide material.
In the present invention, the substrate is protected during cleaning by attaching a pyrolytic carbon coating layer, which is obtained by pyrolysis of polyimide and nanocrystalline cellulose, to the substrate.
In some embodiments, the pyrolytic carbon coating has a thickness of 30-80 μm, such as may be 30, 40, 50, 60, 70, 80 μm and any range between any two values.
In some embodiments, the polyimide is a BTDA-TDI/MDI copolyimide (i.e., a P84 polyimide), such as may be represented by formula (I).
The P84 polyimide may have a relative molecular mass of 80000 to 150000g/mol, such as 80000, 90000, 100000, 110000, 120000, 130000, 140000, 150000g/mol, and any range between any two values, which may be purchased from australian HP polymer GmbH.
The nano microcrystalline cellulose can be purchased commercially or self-made, and the preparation method can be a method conventional in the field, such as an acid hydrolysis method for preparing the nano microcrystalline cellulose.
In some embodiments, the weight ratio of the polyimide to the nanocrystalline cellulose is 1:0.5-2, such as any range that may be 1:0.5, 1:0.8, 1:1, 1:1.2, 1:1.5, 1:1.8, 1:2, and any range between any two values, preferably 1:0.8-1.2.
In some embodiments, the method of preparing a pyrolytic carbon coating further comprises: before the polyimide and the nanocrystalline cellulose are pyrolyzed, the polyimide and the nanocrystalline cellulose are attached to a substrate, and then a curing treatment is performed.
In some embodiments, the conditions of the curing process include: the temperature is 200-400 ℃, such as 200, 220, 240, 260, 280, 300, 320, 340, 360, 380, 400 ℃ and any range between any two values, and the time is 0.5-2h, such as 0.5, 1, 1.5, 2h and any range between any two values.
In some embodiments, the means of attaching comprises: the solution containing polyimide and nanocrystalline cellulose is contacted with a substrate, and then desolvation treatment is performed so that the polyimide and nanocrystalline cellulose are attached to the substrate.
In some embodiments, the concentration of polyimide in the solution is 20-30wt%, such as may be 20, 22, 24, 26, 28, 30wt% and any range between any two values.
In some embodiments, the solvent of the solution is selected from at least one of N-methyl-2-pyrrolidone, N-dimethylformamide, N-dimethylacetamide, and N, N-diethylacetamide.
In the preparation process, the order of addition of the respective substances is not particularly limited as long as a uniform material can be obtained, for example, nanocrystalline cellulose may be added to the solvent first, and then polyimide may be added. The polyimide may be a powder or a particle. During this process, it is also possible to operate with, for example, ultrasound, stirring, etc.
In the present invention, the solvent removal may be performed in a conventional manner in the art, for example, by vacuum drying (for example, drying at 40 to 80 ℃ for 2 to 6 hours under vacuum) or purging with an inert gas (for example, nitrogen), and the like.
In some embodiments, the conditions of pyrolysis include: the pyrolysis temperature is 900-1500 ℃, such as 900, 1000, 1100, 1200, 1300, 1400, 1500 ℃ and any range between any two values, the pyrolysis atmosphere is an inert atmosphere, and the pyrolysis time is 1-3h, such as 1, 1.5, 2, 2.5, 3h and any range between any two values.
In some embodiments, the inert atmosphere is a nitrogen atmosphere, a helium atmosphere, or an argon atmosphere.
In some embodiments, the ramp rate to the pyrolysis temperature is 2-9 ℃/min, such as may be 2, 4, 6, 8, 9 ℃/min, and any range between any two values.
In some embodiments, the concentration of the cleaning gas during cleaning is 80% or more, such as may be 80, 85, 90, 95, 100% and any range between any two values. It should be understood that the gases introduced during the cleaning process include cleaning gases and diluent gases, such as inert gases conventionally used in the art.
In some embodiments, the flow rate of the cleaning gas is 10-100sccm, such as may be 10, 20, 40, 60, 80, 100sccm, and any range between any two values.
In some embodiments, the cleaning process is performed under a nitrogen atmosphere. The flow rate of the nitrogen can be 1-10slm, for example, 1, 2, 4, 6, 8, 10slm and any range between any two values.
In some embodiments, the cleaning conditions include: the temperature is 300-500 ℃, such as 300, 350, 400, 450, 500 ℃ and any range between any two values, and the time is 10-40min, such as 10, 20, 30, 40min and any range between any two values. The pressure may be atmospheric pressure.
Through the above cleaning, silicon carbide on the surface of the pyrolytic carbon film is removed.
In some embodiments, the method further comprises: and (5) annealing the cleaned system.
In some embodiments, the annealing is performed in the presence of nitrogen and oxygen, the oxygen content being less than 0.5%. Compared with nitrogen gas without oxygen, when nitrogen gas with low concentration oxygen is used for annealing, the method can further improve the discharge effect of fluorine atoms, reduce the corrosion of fluorine atoms to the reactor and prolong the service life of the reactor.
In some embodiments, the conditions of the annealing process include: the temperature is 800-1000 ℃, such as 800, 820, 840, 860, 880, 900, 920, 940, 960, 980, 1000 ℃ and any range between any two values, and the time is 10-40min, such as 10, 20, 30, 40min and any range between any two values.
In some embodiments, the total gas flow rate during the annealing process is 1-10slm, such as may be 1, 2, 4, 6, 8, 10slm, and any range between any two values. The total gas flow rate includes a nitrogen flow rate and an oxygen flow rate. And through the annealing process, the fluorine atoms remained in the cleaning process are discharged out of the reactor.
In some embodiments, if the furnace wall surface is significantly yellowish, it is indicative that a substantial portion of the formed silicon carbide film is removed. When the remaining amount of the silicon carbide film formed was found to be significant, further etching was required. After repeating the cleaning operation, the termination of cleaning may be carefully determined based on the apparent color of the substrate.
The technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
The invention is described in detail below in connection with specific embodiments, which are intended to be illustrative rather than limiting.
Preparation example 1
The preparation example is used for explaining the preparation method of the polyimide-nano microcrystalline cellulose pyrolytic carbon film.
N-methyl-pyrrolidone (NMP) is used as a solvent, a proper amount of nano microcrystalline cellulose (NCC) is added, and then P84 polyimide powder is added to obtain a PI/NCC solution, wherein the PI content in the PI/NCC solution is 25wt% and the NCC content in the PI/NCC solution is 20wt%.
Step two: the PI/NCC solution is smeared on the inner wall of a reactor, dried for 4 hours in a vacuum environment at 60 ℃ to volatilize redundant solvent, and then solidified for 1 hour at 300 ℃. N is introduced into the reactor 2 The mixture was incubated at 1000℃for 2 hours to obtain a PI/NCC pyrolytic carbon film of about 40. Mu.m.
Comparative preparation example 1
This preparation example is used to illustrate the preparation method of the reference pyrolytic carbon film.
With methane (CH) 4 ) Is a carbon source precursor, and is prepared by Chemical Vapor Deposition (CVD) process at a deposition temperature of 1000 ℃ and CH 4 The flow rate is 500mL/min, the deposition time is 8h, the deposition pressure is 5kPa, and the deposition pressure is on the inner wall of the reactorThe deposition resulted in a pyrolytic carbon interfacial layer of about 40 μm.
Example 1
This example is used to illustrate a method of cleaning silicon carbide.
This example was conducted in a reactor having a substrate surface coated with a PI/NCC pyrolytic carbon film as described in preparation example 1.
After 15 passes of silicon carbide deposition using the reactor, a cleaning operation was performed under the following specific operating conditions.
(1) Setting the temperature in the furnace to 400 ℃, introducing high-purity nitrogen with the nitrogen flow of 5slm in the heating process under the atmospheric pressure, and then introducing chlorine trifluoride gas for cleaning, wherein the chlorine trifluoride gas flow is 60SCCM, and cleaning for 30min.
(2) Continuously heating to 900 ℃, and introducing a mixed gas of nitrogen and oxygen with the flow rate of 5slm, wherein the mixed gas contains 0.2% of oxygen, and the temperature is kept for 20min.
(3) If the furnace wall surface is significantly yellowish, it is indicated that most of the silicon carbide film formed is removed. When the remaining amount of the silicon carbide film formed was found to be significant, further etching was required. After repeating the cleaning operation, the termination of cleaning is carefully determined according to the apparent color of the base.
After the cleaning was completed, the operation was cycled according to the methods of steps (1) and (2), and no damage was found to the reactor surface after 10 cleaning cycles.
Comparative example 1
This comparative example is used to illustrate the cleaning method of reference silicon carbide.
The operation was performed in accordance with the method of example 1, except that the cleaned deposition furnace was a deposition furnace having the substrate surface covered with the pyrolytic carbon film of comparative preparation example 1, instead of the deposition furnace having the PI/NCC pyrolytic carbon film.
And (3) circularly operating according to the methods of the steps (1) and (2), and cleaning for 6 times to remove the pyrolytic carbon film on the surface of the reactor.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. Furthermore, it should be noted that the scope of the methods and apparatus in the embodiments of the present application is not limited to performing the functions in the order shown or discussed, but may also include performing the functions in a substantially simultaneous manner or in an opposite order depending on the functions involved, e.g., the described methods may be performed in an order different from that described, and various steps may also be added, omitted, or combined. Additionally, features described with reference to certain examples may be combined in other examples.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is to be construed as including any modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (10)
1. A method of cleaning, the method comprising: cleaning a silicon carbide-containing deposit located on a surface of a substrate using a cleaning gas; the substrate comprises a pyrolytic carbon coating on the surface of a base;
the pyrolytic carbon coating is obtained by pyrolysis of polyimide and nano microcrystalline cellulose;
the cleaning gas is chlorine trifluoride.
2. The cleaning method of claim 1, wherein the polyimide is a BTDA-TDI/MDI copolyimide.
3. The cleaning method according to claim 1 or 2, wherein the weight ratio of polyimide to nanocrystalline cellulose is 1:0.5-2, preferably 1:0.8-1.2.
4. The cleaning method according to any one of claims 1 to 3, wherein the preparation method of the pyrolytic carbon coating further comprises: before the polyimide and the nano microcrystalline cellulose are pyrolyzed, the polyimide and the nano microcrystalline cellulose are attached to a substrate, and then the curing treatment is carried out;
preferably, the conditions of the curing treatment include: the temperature is 200-400 ℃ and the time is 0.5-2h.
5. The cleaning method of claim 4, wherein the adhering means comprises: contacting a solution containing polyimide and nanocrystalline cellulose with a substrate, and then performing desolvation treatment so that the polyimide and nanocrystalline cellulose are attached to the substrate;
preferably, the concentration of polyimide in the solution is 20-30wt%;
preferably, the solvent of the solution is selected from at least one of N-methyl-2-pyrrolidone, N-dimethylformamide, N-dimethylacetamide and N, N-diethylacetamide.
6. The cleaning method of any of claims 1-5, wherein the conditions of pyrolysis comprise: the pyrolysis temperature is 900-1500 ℃, the pyrolysis atmosphere is inert atmosphere, and the pyrolysis time is 1-3h;
preferably, the inert atmosphere is a nitrogen atmosphere, a helium atmosphere or an argon atmosphere.
7. The cleaning method according to any one of claims 1 to 6, wherein a concentration of the cleaning gas is 80% or more during cleaning;
preferably, the flow rate of the cleaning gas is 10-100sccm;
preferably, the cleaning process is performed under a nitrogen or argon atmosphere.
8. The cleaning method according to any one of claims 1 to 7, wherein the cleaning conditions include: the temperature is 300-500 ℃ and the time is 10-40min.
9. The cleaning method according to any one of claims 1 to 8, wherein the method further comprises: annealing the cleaned system;
the annealing is performed in the presence of nitrogen and oxygen, the oxygen content being 0.5% or less.
10. The cleaning method of claim 9, wherein the annealing conditions include: the temperature is 800-1000 ℃ and the time is 10-40min; and/or
In the annealing process, the total gas flow rate is 1-10slm.
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