JP6639022B2 - Cleaning method for silicon carbide deposits - Google Patents
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- JP6639022B2 JP6639022B2 JP2016566002A JP2016566002A JP6639022B2 JP 6639022 B2 JP6639022 B2 JP 6639022B2 JP 2016566002 A JP2016566002 A JP 2016566002A JP 2016566002 A JP2016566002 A JP 2016566002A JP 6639022 B2 JP6639022 B2 JP 6639022B2
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 119
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 115
- 238000000034 method Methods 0.000 title claims description 46
- 238000004140 cleaning Methods 0.000 title claims description 42
- 239000007789 gas Substances 0.000 claims description 55
- 229910052731 fluorine Inorganic materials 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 18
- 239000011737 fluorine Substances 0.000 claims description 17
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000010410 layer Substances 0.000 description 54
- 239000010408 film Substances 0.000 description 31
- 238000006243 chemical reaction Methods 0.000 description 28
- 238000005530 etching Methods 0.000 description 27
- 238000005229 chemical vapour deposition Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 239000000523 sample Substances 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000010409 thin film Substances 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000013068 control sample Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- XRURPHMPXJDCOO-UHFFFAOYSA-N iodine heptafluoride Chemical compound FI(F)(F)(F)(F)(F)F XRURPHMPXJDCOO-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002627 tracheal intubation Methods 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 1
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
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Description
本発明は、ＳｉＣエピタキシャル炉内の部材等に堆積した炭化珪素（ＳｉＣ）を含有する堆積物を除去するためのクリーニング方法に関する。 The present invention relates to a cleaning method for removing deposits containing silicon carbide (SiC) deposited on members and the like in a SiC epitaxial furnace.
炭化珪素（ＳｉＣ）は、重要なセラミックス材料として多方面で使用されている。近年、炭化珪素のエピタキシャル成長技術が注目されており、特にその絶縁破壊電圧の高さや高温作動時における信頼性から、低消費電力のトランジスタなどの用途が開発されている。
このような用途に用いられる炭化珪素は、高純度な単結晶である必要がある。大型の炭化珪素単結晶の製造法としては、化学気相堆積法（Ｃｈｅｍｉｃａｌ Ｖａｐｏｒ Ｄｅｐｏｓｉｔｉｏｎ法；ＣＶＤ法）を用いてプロパンガスとシランガスなどの化学反応により膜成長させる方法や、モノメチルシランをＣＶＤ法の原料として膜成長させる方法が知られている。Silicon carbide (SiC) is used in various fields as an important ceramic material. 2. Description of the Related Art In recent years, attention has been paid to silicon carbide epitaxial growth technology. In particular, applications such as low power consumption transistors have been developed because of its high dielectric breakdown voltage and reliability at high temperature operation.
Silicon carbide used for such an application needs to be a high-purity single crystal. As a method for manufacturing a large silicon carbide single crystal, a method of growing a film by a chemical reaction such as a propane gas and a silane gas using a chemical vapor deposition method (Chemical Vapor Deposition method; CVD method), or a method of forming monomethylsilane by a CVD method A method of growing a film as a raw material is known.
これらのＣＶＤ法を用いて、高純度な炭化珪素（ＳｉＣ）単結晶を作製するには、炭化珪素成膜時に、１５００℃以上の高い温度が必要である。そのため、反応容器（ＳｉＣエピタキシャル炉）の内壁やウエハを設置するサセプタなどの装置基材（以下、「部材」と略記することがある。）には、高耐熱性材料である、主としてカーボン母材の表面にＣＶＤ法によって緻密な多結晶のＳｉＣを被覆したもの（ＳｉＣコート）が用いられる。 In order to manufacture a high-purity silicon carbide (SiC) single crystal using these CVD methods, a high temperature of 1500 ° C. or higher is required when forming a silicon carbide film. Therefore, a base material (hereinafter, sometimes abbreviated as “member”) such as an inner wall of a reaction vessel (SiC epitaxial furnace) or a susceptor on which a wafer is placed is mainly a carbon base material which is a high heat-resistant material. (SiC coat) coated with dense polycrystalline SiC by CVD.
また、ＣＶＤ法による膜成長では、反応容器の内壁やサセプタなど意図しない部位にも炭化珪素が付着し、堆積してしまう。それら意図しない部分に堆積した炭化珪素の微粒子（ＳｉＣ堆積物）は、時として剥離、脱落し、炭化珪素薄膜の成長表面に落下して付着し、結晶成長を阻害したり、欠陥を生じさせたりする原因となる。そのため、定期的に反応容器の内壁の堆積した炭化珪素を取り除かなければならない。その除去方法としては、従来、炭化珪素が反応容器の内壁に堆積した場合には、工具を用いて剥離除去するか、容器を定期的に交換する方法が採用されていた。 In the film growth by the CVD method, silicon carbide also adheres to unintended portions such as the inner wall of the reaction vessel and the susceptor, and is deposited. The silicon carbide fine particles (SiC deposits) deposited on those unintended portions sometimes peel off and fall off, fall and adhere to the growth surface of the silicon carbide thin film, and inhibit crystal growth or cause defects. Cause you to Therefore, it is necessary to periodically remove the silicon carbide deposited on the inner wall of the reaction vessel. Conventionally, when silicon carbide has accumulated on the inner wall of the reaction vessel, a method of removing the silicon carbide using a tool or periodically replacing the vessel has been adopted.
堆積した炭化珪素の削り取りや反応容器の交換には長い作業時間を要し、反応器を長期間にわたり大気開放する必要があることから、歩留まりの悪化など生産性にも影響を与える原因となっていた。そのため、装置を開放することなく、無機物質を効率よく除去するガスを用いて、装置内部に付着した炭化珪素を化学的に除去するクリーニング方法が検討されている。 It takes a long working time to remove the deposited silicon carbide and replace the reaction vessel, and it is necessary to open the reactor to the atmosphere for a long period of time. Was. Therefore, a cleaning method for chemically removing silicon carbide adhered to the inside of the device by using a gas that efficiently removes an inorganic substance without opening the device has been studied.
特許文献１（特開２０１４−１５４８６５号公報）には、七フッ化ヨウ素を含むクリーニングガスにより、基材を構成するグラファイトをエッチングして損傷を与えることなく、炭化珪素を含有する堆積物を除去する方法が記載されている。七フッ化ヨウ素ガスは、グラファイトへのダメージを抑え炭化珪素を除去することができる優れたクリーニングガスではあるが、コーティングとして被覆された炭化珪素とその上に堆積した炭化珪素(堆積物)との反応選択性に乏しいという問題がある。また、特許文献１には、より一般的なエッチングガスであるフッ素ガス（Ｆ2）がクリーニングガスとして不適であることを示す比較例が記載されている。Patent Document 1 (Japanese Patent Application Laid-Open No. 2014-154865) discloses that a cleaning gas containing iodine heptafluoride removes deposits containing silicon carbide without etching and damaging graphite constituting a base material. A method is described. Iodine heptafluoride gas is an excellent cleaning gas that can suppress damage to graphite and remove silicon carbide.However, silicon carbide coated as a coating and silicon carbide (deposit) deposited on it There is a problem that reaction selectivity is poor. Patent Document 1 describes a comparative example showing that fluorine gas (F 2 ), which is a more general etching gas, is not suitable as a cleaning gas.
窒素ガスなどの不活性ガスで希釈したフッ素ガスによるクリーニングのデータが示されていない特許文献１の記載内容から、仮に窒素ガス（Ｎ2）などで希釈したフッ素ガスを用いた場合に、グラファイト等のカーボン母材に予め被覆された炭化珪素へダメージを与えることなく、材質のダメージが抑えられ、ＳｉＣエピタキシャル炉内の部材に堆積した炭化珪素（ＳｉＣ）を含有する堆積物のみを選択的に除去できることは当業者には予測困難であると考えられる。According to the description in Patent Document 1 which does not show data on cleaning with fluorine gas diluted with an inert gas such as nitrogen gas, if fluorine gas diluted with nitrogen gas (N 2 ) or the like is used, graphite or the like is used. Damage to the material is suppressed without damaging the silicon carbide previously coated on the carbon base material, and only deposits containing silicon carbide (SiC) deposited on members in the SiC epitaxial furnace are selectively removed. What can be done is considered difficult to predict by those skilled in the art.
特許文献２（特開２０１３−２５１４８７号公報）には、予めプラズマ化された三フッ化窒素等のフッ素含有ガスにより炭化珪素よりなる付着物を除去する方法が示されている。
特許文献２では、プラズマ状態のガスを用いるため、プラズマを発生させるために特別な装置が必要になる。また、炭化珪素よりなる堆積物以外の部材、特にカーボン母材の表面にＣＶＤ法によって緻密な多結晶のＳｉＣを被覆したもの（ＳｉＣコート）へのダメージを防ぐことは困難であった。Patent Literature 2 (Japanese Patent Application Laid-Open No. 2013-251487) discloses a method for removing deposits made of silicon carbide using a fluorine-containing gas such as nitrogen trifluoride that has been made into plasma in advance.
In Patent Literature 2, since a gas in a plasma state is used, a special device is required to generate plasma. Further, it has been difficult to prevent damage to members other than the deposit made of silicon carbide, particularly those in which the surface of a carbon base material is coated with dense polycrystalline SiC by a CVD method (SiC coat).
本発明の目的は、より一般的なエッチングガスであるフッ素ガス（Ｆ2）を用いて、カーボン母材の表面にＣＶＤ法によって緻密な多結晶のＳｉＣを被覆（コート）された基材に堆積した炭化珪素を含有する堆積物のクリーニング処理において、緻密な多結晶のＳｉＣコートに損傷を与えることなく、十分なクリーニング速度でＳｉＣ堆積物を除去できる方法を提供することにある。An object of the present invention is to deposit fluorine-containing gas (F 2 ), which is a more general etching gas, on a substrate in which dense polycrystalline SiC is coated (coated) on the surface of a carbon base material by a CVD method. It is an object of the present invention to provide a method capable of removing a SiC deposit at a sufficient cleaning rate without damaging a dense polycrystalline SiC coat in a cleaning process of a deposited silicon carbide-containing deposit.
本発明者らは、上記の課題を解決すべく鋭意検討した結果、不活性ガスで希釈されたフッ素ガスを、特定範囲の濃度でかつ特定の温度範囲の条件で流通させることにより、緻密な多結晶のＳｉＣで被覆された基材を損傷することなく、炭化珪素含有堆積物を優先的に除去できることを見出し本発明を完成した。
すなわち、本発明は以下の［１］〜［４］の炭化珪素堆積物のクリーニング方法及び［５］の炭化珪素結晶の製造方法に関する。
［１］炭化珪素でコートされた部材に堆積した炭化珪素堆積物に対し、フッ素ガス１〜２０体積％と不活性ガス８０〜９９体積％とからなる混合ガスを、２００〜５００℃の温度にてノンプラズマ状態で流通させることを特徴とする炭化珪素堆積物のクリーニング方法。
［２］不活性ガスが、窒素ガス、アルゴンガス、ヘリウムガス及び空気から選択される前項１に記載の炭化珪素堆積物のクリーニング方法。
［３］不活性ガスが窒素ガスまたはアルゴンガスである前項２に記載の炭化珪素堆積物のクリーニング方法。
［４］前記炭化珪素でコートされた部材が、炭化珪素エピタキシャル炉を構成する部材である前項１〜３のいずれか１項に記載の炭化珪素堆積物のクリーニング方法。
［５］前項４の方法でクリーニングされた炭化珪素エピタキシャル炉を使用することを特徴とする炭化珪素結晶の製造方法。The present inventors have conducted intensive studies in order to solve the above-mentioned problems, and as a result, by allowing a fluorine gas diluted with an inert gas to flow at a concentration in a specific range and under a condition of a specific temperature range, a dense multi-layer gas has been developed. The present inventors have found that silicon carbide-containing deposits can be preferentially removed without damaging a substrate coated with crystalline SiC, and completed the present invention.
That is, the present invention relates to the following silicon carbide deposit cleaning methods [1] to [4] and the silicon carbide crystal manufacturing method [5].
[1] A mixed gas consisting of 1 to 20% by volume of a fluorine gas and 80 to 99% by volume of an inert gas is heated to a temperature of 200 to 500 ° C. with respect to the silicon carbide deposit deposited on the member coated with silicon carbide. A method for cleaning silicon carbide deposits, wherein the method is carried out in a non-plasma state.
[2] The method for cleaning a silicon carbide deposit according to the above item 1, wherein the inert gas is selected from nitrogen gas, argon gas, helium gas and air.
[3] The method for cleaning a silicon carbide deposit according to item 2, wherein the inert gas is a nitrogen gas or an argon gas.
[4] The method for cleaning a silicon carbide deposit according to any one of the above items 1 to 3, wherein the member coated with silicon carbide is a member constituting a silicon carbide epitaxial furnace.
[5] A method for producing a silicon carbide crystal, comprising using a silicon carbide epitaxial furnace cleaned by the method according to the above item 4.
本発明の方法によれば、ＳｉＣエピタキシャル成長炉におけるＳｉＣコートされたチャンバー内の部材を損傷することなく、ＳｉＣ堆積物を容易に除去することができる。 According to the method of the present invention, the SiC deposit can be easily removed without damaging the members in the SiC coated chamber in the SiC epitaxial growth furnace.
以下、本発明に係る炭化珪素堆積物のクリーニング方法を詳細に説明する。
本発明の適用対象となる堆積物は、堆積物の主成分として炭化珪素を含んでいれば特に限定されるものではなく、炭化珪素を単独成分とするものでもよい。具体的には、化学的気相堆積法（ＣＶＤ法）、有機金属気相成長法（ＭＯＣＶＤ法）、スパッタリング法、ゾルゲル法、蒸着法等の方法を用いて薄膜、厚膜、粉体、ウイスカ等を製造する際に、製造装置の内壁または半導体ウエハを設置するためのサセプタなどの冶具、配管等の付属装置に付随的に堆積した不要な堆積物である。Hereinafter, the method for cleaning silicon carbide deposits according to the present invention will be described in detail.
The deposit to which the present invention is applied is not particularly limited as long as it contains silicon carbide as a main component of the deposit, and may be silicon carbide as a sole component. Specifically, a thin film, a thick film, a powder, a whisker are formed by using a method such as a chemical vapor deposition method (CVD method), a metal organic chemical vapor deposition method (MOCVD method), a sputtering method, a sol-gel method, and a vapor deposition method. Unnecessary deposits that accumulate on an inner wall of a manufacturing apparatus, a jig such as a susceptor for installing a semiconductor wafer, and an auxiliary device such as a pipe when manufacturing a semiconductor device.
また、炭化珪素の薄膜、厚膜等のみではなく六方晶ＳｉＣウエハなどの大型バルク結晶成長を行う方法、例えば、特開２００４−２２４６６３号公報（特許文献３）に開示されている、炭化珪素の原料を加熱昇華させて種結晶上に炭化珪素の結晶成長を行い大型バルク結晶成長させる昇華再結晶法（改良レリー法）を実施する製造装置の内壁またはその付属部品に付着した不要な堆積物にも適用可能である。 In addition, a method for growing a large bulk crystal such as a hexagonal SiC wafer as well as a thin film and a thick film of silicon carbide, for example, a method of silicon carbide disclosed in Japanese Patent Application Laid-Open No. 2004-224663 (Patent Document 3). Unnecessary deposits adhering to the inner wall of the manufacturing equipment or its attached parts that perform the sublimation recrystallization method (improved Lerry method) in which the raw material is heated and sublimated to grow silicon carbide on the seed crystal and grow large bulk crystals Is also applicable.
本発明方法の適用対象となる装置の基材は、カーボン母材表面の少なくとも一部を炭化珪素などの保護膜で被覆した１５００℃以上の高温条件に耐えうる基材である。
具体的には、上述の炭化珪素の製造装置を構成する物品、炭化珪素製造装置の内壁、及び半導体ウエハを設置するためのサセプタなどの冶具、配管等の付属装置を挙げることができる。すなわち、本発明のクリーニング方法は、不要な堆積物が堆積しやすい製造装置の内壁、半導体ウエハを設置するためのサセプタ、半導体デバイス、コーティング工具などの薄膜を形成する炭化珪素製膜装置やウイスカ、粉末などを製造する炭化珪素製造装置の内壁、及び前記装置の付属部品に堆積したＳｉＣ堆積物の除去に適用できる。また、炭化珪素の薄膜、厚膜等のみでなく六方晶ＳｉＣウエハなどの大型バルク結晶成長を行う製造装置の内壁またはその付属部品に付着した不要なＳｉＣ堆積物の除去にも適用可能である。これらのうち、成膜装置への適用が好ましく、特に、高温条件での成膜が行われる炭化珪素のエピタキシャル膜成長を行う製膜装置の内壁またはその付属部品に堆積したＳｉＣ堆積物への適用がさらに好ましい。これらの中でも、不要な堆積物が堆積しやすい製造装置の内壁及び半導体ウエハを設置するためのサセプタへの適用が特に好適である。The base material of the apparatus to which the method of the present invention is applied is a base material in which at least a part of the surface of the carbon base material is coated with a protective film such as silicon carbide and can withstand a high temperature condition of 1500 ° C. or more.
Specifically, there can be mentioned an article constituting the above-described silicon carbide manufacturing apparatus, an inner wall of the silicon carbide manufacturing apparatus, a jig such as a susceptor for installing a semiconductor wafer, and an attached device such as a pipe. That is, the cleaning method of the present invention is an inner wall of a manufacturing apparatus on which unnecessary deposits are easily deposited, a susceptor for installing a semiconductor wafer, a semiconductor device, a silicon carbide film forming apparatus and a whisker for forming a thin film such as a coating tool, The present invention can be applied to the removal of SiC deposits deposited on the inner wall of a silicon carbide manufacturing apparatus for manufacturing powder and the like, and on an accessory part of the apparatus. Further, the present invention can be applied not only to the removal of unnecessary SiC deposits adhering to the inner wall of a manufacturing apparatus for growing a large-sized bulk crystal such as a hexagonal SiC wafer but also to its attached parts, as well as a thin film and a thick film of silicon carbide. Among these, application to a film forming apparatus is preferable, and in particular, application to an SiC deposit deposited on an inner wall of a film forming apparatus for performing epitaxial film growth of silicon carbide which is formed under a high temperature condition or an accessory thereof. Is more preferred. Among these, application to a susceptor for installing an inner wall of a manufacturing apparatus and a semiconductor wafer on which unnecessary deposits are easily deposited is particularly preferable.
本発明の方法では、特定の濃度範囲に希釈したフッ素ガスを用いて、上述の基材を反応器に設置したヒーターで特定の温度範囲に加熱しながら基材の表面に形成されている炭化珪素を含有する堆積物を選択的に除去する。基材に堆積した不要な堆積物が本発明の方法により除去される機構としては、フッ素の熱分解によって生じたフッ素ラジカルが堆積物中の炭化珪素と反応してＳｉＦ4、ＣＦ4となることにより除去されると考えられる。In the method of the present invention, using a fluorine gas diluted to a specific concentration range, silicon carbide formed on the surface of the substrate while heating the above-described substrate to a specific temperature range with a heater installed in a reactor Is selectively removed. The mechanism by which unnecessary deposits deposited on the substrate are removed by the method of the present invention is that fluorine radicals generated by thermal decomposition of fluorine react with silicon carbide in the deposits to form SiF 4 and CF 4. Is considered to be removed.
内壁に付着するＳｉＣ膜は、内壁を構成する緻密な多結晶のＳｉＣ膜（ＳｉＣコート膜）とは異なり、緻密でない多結晶の膜と考えられる。ＳｉＣコート膜は灰色で表面が滑らかであるのに対し、堆積物は黄色であり、肉眼でも細かな粒子の集合体であることが確認できる。表面粗さで示すとコート膜の表面粗さがＲａ≦４であるのに対し、堆積物の表面粗さはＲａ≧１０である。
この緻密でない多結晶のＳｉＣ膜のエッチングレートは、緻密な多結晶のＳｉＣ膜に比較して十分速くなると予想されるが、１００％のＦ2ガスを用いた場合には、同一成分であるコート膜と堆積物のエッチングレートには堆積物が選択的に除去されるほどの差は生じない（特許文献３）。The SiC film adhering to the inner wall is considered to be a non-dense polycrystalline film unlike the dense polycrystalline SiC film (SiC coat film) constituting the inner wall. While the SiC coat film is gray and has a smooth surface, the deposit is yellow and the naked eye can confirm that it is an aggregate of fine particles. In terms of surface roughness, the surface roughness of the coating film is Ra ≦ 4, whereas the surface roughness of the deposit is Ra ≧ 10.
It is expected that the etching rate of the non-dense polycrystalline SiC film will be sufficiently faster than that of the dense polycrystalline SiC film. However, when 100% F 2 gas is used, the coating rate of the same component is reduced. There is no difference between the etching rates of the film and the deposit such that the deposit is selectively removed (Patent Document 3).
そこで、本発明者らは、Ｆ2ガスを不活性ガスで希釈した混合ガスをエッチングガスとする方法について検討した。そして、フッ素濃度が１〜２０体積％、好ましくは５〜１５％の範囲で、十分なエッチングレート差が得られることを確認した。この濃度範囲に希釈したＦ2ガスを用いることにより、緻密な多結晶のＳｉＣ膜と、緻密でない多結晶のＳｉＣ膜との間のエッチングレートに明確な差が認められる。すなわち、エッチングレートの差を利用することにより、内壁を構成するＳｉＣ膜を実質的にエッチングすることなく、内壁に付着したＳｉＣ膜をエッチング除去することができる。Therefore, the present inventors have studied a method of using a mixed gas obtained by diluting F 2 gas with an inert gas as an etching gas. Then, it was confirmed that a sufficient etching rate difference was obtained when the fluorine concentration was in the range of 1 to 20% by volume, preferably 5 to 15%. By using the F 2 gas diluted to this concentration range, a clear difference is observed in the etching rate between the dense polycrystalline SiC film and the non-dense polycrystalline SiC film. That is, by utilizing the difference in the etching rates, the SiC film adhering to the inner wall can be removed by etching without substantially etching the SiC film forming the inner wall.
本発明で使用する不活性ガスは特に限定されるものではないが、窒素ガス（Ｎ2）、アルゴンガス（Ａｒ）、ヘリウムガス（Ｈｅ）、及び空気が挙げられる。これらの中でもＮ2及びＡｒが好ましい。The inert gas used in the present invention is not particularly limited, but includes nitrogen gas (N 2 ), argon gas (Ar), helium gas (He), and air. Among them, N 2 and Ar are preferable.
クリーニングの反応条件に関しては、反応温度は炭化珪素を含む堆積物が堆積した基材の温度を２００〜５００℃、好ましくは２５０〜３５０℃の範囲に設定する。２００℃より低い温度では十分なクリーニング性能が得られない場合がある。５００℃より高い温度の場合、エッチングレートの差が少なくなるだけでなく、エネルギーの無駄になり消費電力などランニングコストが高くなる。 Regarding the cleaning reaction conditions, the reaction temperature is set to a temperature of the substrate on which the deposit containing silicon carbide is deposited, in the range of 200 to 500 ° C, preferably 250 to 350 ° C. If the temperature is lower than 200 ° C., sufficient cleaning performance may not be obtained. When the temperature is higher than 500 ° C., not only the difference in etching rate is reduced, but also energy is wasted and running costs such as power consumption are increased.
反応温度は反応器に設置されたヒーターにより制御される。ヒーターとしては装置全体を温める加熱器を用いてもよいし、加熱ターゲット部材のみを温めてその伝熱により付着物を温めるような加熱器を用いてもよい。センサーは付着物付近に設置する。センサーを直接ガスに接触させられない場合には、内挿管等を用いてもよい。 The reaction temperature is controlled by a heater installed in the reactor. As the heater, a heater that heats the entire apparatus may be used, or a heater that heats only the heating target member and heats the deposit by heat transfer may be used. The sensor is installed near the deposit. When the sensor cannot be brought into direct contact with the gas, an intubation tube or the like may be used.
反応の圧力については、特に制限されるものではない。通常は大気圧下で行うが、−０．０５〜０．３ＭＰａＧが適用可能である。
クリーニングガスの流量は、クリーニング装置の反応器容量により適宜調整されるが、線速度（ＬＶ）として、ＬＶ＝０．１〜１０ｍ／ｍｉｎが好ましい。The reaction pressure is not particularly limited. Usually, it is performed under atmospheric pressure, but -0.05 to 0.3 MPaG can be applied.
The flow rate of the cleaning gas is appropriately adjusted depending on the reactor capacity of the cleaning device, and the linear velocity (LV) is preferably LV = 0.1 to 10 m / min.
本発明のクリーニング方法は、ＣＶＤ法により半導体デバイス、コーティング工具などの薄膜を形成する炭化珪素製膜装置やウイスカ、粉末などを製造する炭化珪素製造装置の内壁及び前記装置の付属部品に堆積したＳｉＣ堆積物の除去に適用できる。また、炭化珪素の薄膜、厚膜等のみでなく六方晶ＳｉＣウエハなどの大型バルク結晶成長を行う製造装置の内壁またはその付属部品に付着した不要なＳｉＣ堆積物の除去にも適用可能である。これらのうち、成膜装置への適用が好ましく、特に、高温条件での成膜が行われる炭化珪素のエピタキシャル膜成長を行う製膜装置の内壁またはその付属部品に堆積したＳｉＣ堆積物の除去への適用が好ましい。 The cleaning method of the present invention is a method for forming a thin film such as a semiconductor device and a coating tool by a CVD method, a silicon carbide film forming apparatus for forming a thin film, a whisker, and a silicon carbide manufacturing apparatus for manufacturing powders. Applicable for removing sediment. Further, the present invention can be applied not only to the removal of unnecessary SiC deposits adhering to the inner wall of a manufacturing apparatus for growing a large-sized bulk crystal such as a hexagonal SiC wafer but also to its attached parts, as well as a thin film and a thick film of silicon carbide. Among these, application to a film forming apparatus is preferable, and particularly, to removal of SiC deposits deposited on an inner wall of a film forming apparatus for performing epitaxial film growth of silicon carbide which is formed under a high temperature condition or an accessory part thereof. Is preferred.
以下、実施例及び比較例により、本発明を説明するが、本発明はこれらの実施例により限定されるものではない。
クリーニング装置として、図１に示す円筒形の反応管１（ニッケル製）を備えた外熱式縦型反応炉を使用した。円筒形の反応管１には、クリーニングガスを供給するフッ素ガス供給部２と希釈用ガス供給部３が接続されており、反応管１の下流には、ガスを反応管から排出する排気部４が設けられている。さらに、反応管１の外周部には外部ヒーターとして誘導加熱コイル５が設置され、この誘導コイルによって反応管の内部を加熱することができる構成とした。クリーニング試験は、サンプル７（評価用サンプルと対照サンプル）を反応管内部の裁置台６に設置して行った。Hereinafter, the present invention will be described with reference to Examples and Comparative Examples, but the present invention is not limited to these Examples.
As the cleaning device, an externally heated vertical reactor equipped with a cylindrical reaction tube 1 (made of nickel) shown in FIG. 1 was used. A fluorine gas supply unit 2 for supplying a cleaning gas and a dilution gas supply unit 3 are connected to the cylindrical reaction tube 1, and an exhaust unit 4 for discharging gas from the reaction tube is provided downstream of the reaction tube 1. Is provided. Furthermore, an
実施例１：
カーボン母材にＳｉＣコートされたチャンバー内部材を有するＳｉＣエピタキシャル炉でＳｉＣエピタキシャル成長工程を繰り返し行い、ＳｉＣ堆積物が堆積したチャンバー内部材を５ｍｍ角の大きさに切り出し、評価用サンプルとした。また、ＳｉＣエピタキシャル成長工程を行い（堆積物が堆積していない）ＳｉＣコートされたチャンバー内部材から１ｃｍ角の大きさの対照サンプルを切り出した。なお、対照サンプルではコート膜が灰色で表面が滑らかであるのに対し、評価用サンプルでは、堆積物は黄色で細かな粒子の集合体であり、両者の違いは肉眼で確認できるが、断面をＳＥＭ（Scanning Electron Microscope）観察した結果、図２（Ａ）に示すように、ＳｉＣコートの厚みはいずれも７０μｍ、評価用サンプルの堆積物（デポ）の厚みはおよそ２５０μであった。Example 1
The SiC epitaxial growth process was repeated in a SiC epitaxial furnace having a chamber member in which a carbon base material was coated with SiC, and the chamber member on which the SiC deposit had been deposited was cut into a size of 5 mm square to obtain a sample for evaluation. In addition, a control sample having a size of 1 cm square was cut out from a member in the chamber coated with SiC by performing a SiC epitaxial growth step (no deposit was deposited). In the control sample, the coating film was gray and the surface was smooth, whereas in the evaluation sample, the deposit was a collection of fine yellow particles, and the difference between the two could be confirmed with the naked eye. As a result of SEM (Scanning Electron Microscope) observation, as shown in FIG. 2A, the thickness of each SiC coat was 70 μm, and the thickness of the deposit (depot) of the evaluation sample was about 250 μm.
これら２つのサンプルを、図１に示す内挿管を有するニッケル（Ｎｉ）製の反応管（φ３／４インチ、長さ３０ｍｍ）内の中心位置のサンプル裁置台に設置した。内挿管内のサンプル設置場所付近に熱電対を設置した。
反応管を、電気炉を用いて２８０℃に加熱し、大気圧条件下、Ｆ2濃度１０体積％、Ｎ2濃度９０体積％のガスを線速度（ＬＶ）１ｍ／ｍｉｎとなるよう、流量１８０ｍｌ／ｍｉｎで６０分間流通させた。その結果、堆積物層は２１０μｍまで減少したが、ＳｉＣコート層は７０μｍを保っていた（図２（Ｂ））。
エッチングレートは、堆積物層については０．６７μｍ／ｍｉｎ、コート層については＜０．０８μｍ／ｍｉｎであり、コート層に対する堆積物層のエッチングレート比は＞８．４であった。These two samples were set on a sample placing table at the center position in a nickel (Ni) reaction tube (φ3 / 4 inch, length 30 mm) having an inner tube shown in FIG. A thermocouple was installed near the sample installation location in the intubation.
The reaction tube was heated to 280 ° C. using an electric furnace, and a gas having an F 2 concentration of 10% by volume and a N 2 concentration of 90% by volume was supplied at a flow rate of 180 ml so that the linear velocity (LV) was 1 m / min. / Min for 60 minutes. As a result, the deposit layer was reduced to 210 μm, while the SiC coat layer was maintained at 70 μm (FIG. 2 (B)).
The etch rate was 0.67 μm / min for the deposit layer, <0.08 μm / min for the coat layer, and the etch rate ratio of the deposit layer to the coat layer was> 8.4.
実施例２：
ガスの流通時間を３５０分間としたこと以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は消失したがＳｉＣコートの厚みは６５μｍであった（図２（Ｃ））。
エッチングレートは、堆積物層については０．７１μｍ／ｍｉｎ、コート層については０．０１４μ／ｍｉｎであり、コート層に対する堆積物層のエッチングレート比は５１であった。Example 2:
A cleaning test was performed under the same conditions as in Example 1 except that the gas flow time was 350 minutes. As a result, the deposit layer disappeared, but the thickness of the SiC coat was 65 μm (FIG. 2C).
The etching rate was 0.71 μm / min for the deposit layer, 0.014 μ / min for the coat layer, and the etching rate ratio of the deposit layer to the coat layer was 51.
実施例３：
ガス組成をＦ2濃度５体積％、Ｎ2濃度９５体積％とした以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は２２０μｍまで減少したが、ＳｉＣコート層は７０μｍを保っていた。
エッチングレートは、堆積物層については０．５０μｍ／ｍｉｎ、コート層については＜０．０８μｍ／ｍｉｎであり、コート層に対する堆積物層のエッチングレート比は＞６．３であった。Example 3
A cleaning test was performed under the same conditions as in Example 1 except that the gas composition was changed to an F 2 concentration of 5% by volume and an N 2 concentration of 95% by volume. As a result, the deposit layer was reduced to 220 μm, but the SiC coat layer maintained 70 μm.
The etch rate was 0.50 μm / min for the deposit layer, <0.08 μm / min for the coat layer, and the etch rate ratio of the deposit layer to the coat layer was> 6.3.
実施例４：
ガス組成をＦ2濃度１５体積％、Ｎ2濃度８５体積％とした以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は１９０μｍまで減少したが、ＳｉＣコート層は６５μｍまでの減少に留まった。
エッチングレートは、堆積物層については１０μｍ／ｍｉｎ、コート層については０．８３μｍ／ｍｉｎであり、コート層に対する堆積物層のエッチングレート比は１２であった。Example 4:
A cleaning test was performed under the same conditions as in Example 1 except that the gas composition was changed to an F 2 concentration of 15% by volume and an N 2 concentration of 85% by volume. As a result, the deposit layer was reduced to 190 μm, but the SiC coat layer was reduced to only 65 μm.
The etching rate was 10 μm / min for the deposit layer, 0.83 μm / min for the coat layer, and the etching rate ratio of the deposit layer to the coat layer was 12.
実施例５：
反応管の温度を４００℃にした以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は１９０μｍまで減少したが、ＳｉＣコート層は６５μｍまでの減少に留まった。
エッチングレートは、堆積物層については１０μｍ／ｍｉｎ、コート層については０．８３μｍ／ｍｉｎであり、コート層に対する堆積物層のエッチングレート比は１２であった。Example 5:
A cleaning test was performed under the same conditions as in Example 1 except that the temperature of the reaction tube was set to 400 ° C. As a result, the deposit layer was reduced to 190 μm, but the SiC coat layer was reduced to only 65 μm.
The etching rate was 10 μm / min for the deposit layer, 0.83 μm / min for the coat layer, and the etching rate ratio of the deposit layer to the coat layer was 12.
比較例１：
反応管の温度を５５０℃にした以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は２００μｍまで減少し、ＳｉＣコート層も５０μｍまで減少した。
エッチングレートは、堆積物層については０．８３／ｍｉｎ、コート層については０．１７μｍ／ｍｉｎであり、コート層に対する堆積物層のエッチングレート比は４．９であった。Comparative Example 1:
A cleaning test was performed under the same conditions as in Example 1 except that the temperature of the reaction tube was set to 550 ° C. As a result, the deposit layer was reduced to 200 μm, and the SiC coat layer was also reduced to 50 μm.
The etching rate was 0.83 / min for the deposit layer and 0.17 μm / min for the coat layer, and the etching rate ratio of the deposit layer to the coat layer was 4.9.
比較例２：
反応管の温度を１５０℃にした以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は２５０μｍのまま変化せず、ＳｉＣコート層も７０μｍのまま変化しなかった。Comparative Example 2:
A cleaning test was performed under the same conditions as in Example 1 except that the temperature of the reaction tube was set to 150 ° C. As a result, the deposit layer remained unchanged at 250 μm, and the SiC coat layer remained unchanged at 70 μm.
比較例３：
ガス組成をＦ2濃度３０体積％、Ｎ2濃度７０体積％とした以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は２１０μｍまで減少し、ＳｉＣコート層も５０μｍまで減少した。
エッチングレートは、堆積物層については０．６７μｍ／ｍｉｎ、コート層については０．１７μｍ／ｍｉｎであり、コート層に対する堆積物層のエッチングレート比は３．９であった。Comparative Example 3:
A cleaning test was performed under the same conditions as in Example 1 except that the gas composition was changed to an F 2 concentration of 30% by volume and an N 2 concentration of 70% by volume. As a result, the deposit layer was reduced to 210 μm, and the SiC coat layer was also reduced to 50 μm.
The etching rate was 0.67 μm / min for the deposit layer and 0.17 μm / min for the coat layer, and the etching rate ratio of the deposit layer to the coat layer was 3.9.
比較例４：
ガス組成をＦ2濃度体積０．５％、Ｎ2濃度９９．５体積％とした以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は２５０μｍのまま変化せず、ＳｉＣコート層も７０μｍのまま変化しなかった。Comparative Example 4:
A cleaning test was performed under the same conditions as in Example 1 except that the gas composition was changed to an F 2 concentration volume of 0.5% and an N 2 concentration of 99.5 volume%. As a result, the deposit layer remained unchanged at 250 μm, and the SiC coat layer remained unchanged at 70 μm.
比較例５：
反応管の前段にプラズマ発生部を設け、クリーニングガスを予めプラズマ状態としてから反応管に導入した。プラズマ発生部には２．４５ＧＨｚ（印加電力１０００Ｗ）のプラズマ発生器を用いた。また、ガス組成はＦ2濃度１０体積％、Ａｒ濃度９０体積％とした。それ以外は実施例１と同じ条件にてクリーニング試験を行った。その結果、堆積物層は２１０μｍまで減少し、ＳｉＣコート層も５０μｍまで減少した。
エッチングレートは、堆積物層については０．６７μｍ／ｍｉｎ、コート層については０．１７μｍ／ｍｉｎであり、コート層に対する堆積物層のエッチングレート比は３．９であった。Comparative Example 5:
A plasma generating section was provided at a stage preceding the reaction tube, and the cleaning gas was brought into a plasma state in advance and then introduced into the reaction tube. A 2.45 GHz (applied power: 1000 W) plasma generator was used for the plasma generator. The gas composition was set to an F 2 concentration of 10% by volume and an Ar concentration of 90% by volume. Otherwise, a cleaning test was performed under the same conditions as in Example 1. As a result, the deposit layer was reduced to 210 μm, and the SiC coat layer was also reduced to 50 μm.
The etching rate was 0.67 μm / min for the deposit layer and 0.17 μm / min for the coat layer, and the etching rate ratio of the deposit layer to the coat layer was 3.9.
実施例及び比較例の結果を表１にまとめて示す。
表１より、フッ素ガス１〜２０体積％と不活性ガス８０〜９９体積％とからなる混合ガスを、２００〜５００℃の温度で流通させることにより堆積物層とコート層のエッチングレート比を大きくすることができ、堆積物を優先的にクリーニングできることがわかる。そして、フッ素ガス濃度、及び反応温度のどちらかが上記範囲外である条件では、堆積物のクリーニングが行えないか、エッチングレート比が小さくなりコート層へダメージを与えてしまう。また、フッ素ガス濃度、反応温度が上記範囲内であっても、プラズマ条件下ではエッチングレート比が小さくなりコート層へダメージを与えてしまうことがわかる。 As shown in Table 1, by flowing a mixed gas consisting of 1 to 20% by volume of fluorine gas and 80 to 99% by volume of inert gas at a temperature of 200 to 500 ° C., the etching rate ratio between the deposit layer and the coat layer is increased. It can be seen that the deposit can be preferentially cleaned. If either the fluorine gas concentration or the reaction temperature is out of the above range, the deposit cannot be cleaned, or the etching rate ratio becomes small and the coating layer is damaged. Further, it can be seen that even when the fluorine gas concentration and the reaction temperature are within the above ranges, the etching rate ratio becomes small under plasma conditions, and the coating layer is damaged.
１ 反応管
２ フッ素ガス供給部
３ 希釈用ガス供給部
４ 排気部
５ 誘導加熱コイル
６ サンプル裁置台
７ サンプルReference Signs List 1 reaction tube 2 fluorine gas supply unit 3 dilution gas supply unit 4
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