TW200811320A - Single crystal SiC, and method for producing the same - Google Patents

Single crystal SiC, and method for producing the same Download PDF

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Publication number
TW200811320A
TW200811320A TW96116795A TW96116795A TW200811320A TW 200811320 A TW200811320 A TW 200811320A TW 96116795 A TW96116795 A TW 96116795A TW 96116795 A TW96116795 A TW 96116795A TW 200811320 A TW200811320 A TW 200811320A
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Taiwan
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single crystal
sic
crystal sic
particles
producing
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TW96116795A
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Chinese (zh)
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Shoji Akiyama
Masanori Ikari
Takao Abe
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Shinetsu Chemical Co
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/14—Feed and outlet means for the gases; Modifying the flow of the reactive gases
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02367—Substrates
    • H01L21/0237—Materials
    • H01L21/02373—Group 14 semiconducting materials
    • H01L21/02378—Silicon carbide
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02524—Group 14 semiconducting materials
    • H01L21/02529—Silicon carbide
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/02634—Homoepitaxy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Power Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Computer Hardware Design (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)

Abstract

This invention provides an improved method for epitaxially growing single crystal SiC stably for a long time, and provides the resulting high-quality single crystal SiC. This invention provides a method for producing single crystal SiC, characterized by including a step of arranging, within a crucible, a susceptor mounted with SiC seed crystals, and a raw material supply tube for supplying raw materials, such as SiO2 particles and carbon (C) particles, for producing single crystal SiC; and a step of growing the single crystal SiC, by supplying the raw materials for producing the single crystal SiC together with an inert carrier gas through the raw material supply tube onto SiC seed crystals within the crucible that is set to a high temperature atmosphere; wherein a supplying mole ratio of SiO2 to C (SiO2:C), among the raw materials, is 1.05:3.0 to 2.0:3.0. This invention also provides the single crystal SiC produced by the above production method.

Description

200811320 九、發明說明： 【發明所屬之技術領域】 用之導體元件用材料或led用材料而利 【先前技術】 由於單結晶SiC其結晶的結合能強，絕緣破壞電場大曰 導熱係數高，因此作為雜苛環境用元件或功率元件用 相當有效益的。除此之外，由於其晶格常數接近GaN 化^ 的晶J常數’因此作為GaN-LED用峨反材料而言也非；有 傳統士，此種單結晶SiC的製造方式包括：在石墨掛J SiC粉末昇華，在石墨掛塥的内壁使單彡士 / (Ka^Me.0.) ; «^^1'；； 布最仏化’然後於使其再結晶化的部分配置沉種單姓日^ ΪΪίίί^θ的改良式瑞里法；將氣體源藉由 化學反應’ 一邊進行磊晶成長的CVD法；以及在石墨產生 , ^sic^slCi 件Γ第ί章fr 晶的昇華接近法等（請參考非專利文 法，S 而言’上述所介紹的各種單結晶SiC的製造方 "φ 疋那一種，都仍然各自有其問題存在。首先，在盘¥本 以自造結晶性良好的單結晶sic，但是因為這ΐ重方式ΐ =狀控制以及結晶面控制，一方^^ 到大數以左右的高速得 式進臟献，输 200811320 的問題。 而在CVD法巾，__製造高純度且低缺陷 但是因為此種製造法係以稀薄的氣體源進貝早 ，此，長晶速度較慢，成長速紐為1Q/zm/h以下Βθ成長’ 無法得到長形的單結晶SiC鑄錠的問題。 王又，且有 在昇華接近法巾，_能夠以摘比較簡單 ==二:結構上的 碳超二 晶上以碳將二氧化矽還原的方法。而 種早、、、。 =ίί=ί^Γ。高速獲得高品f的單結晶^且欠 於豆3述=ΐ件1所揭露的單結晶Sic之製造方法中，關 —法、·供應綠、環魏體調整;r法等裝置 的各種結構，亚無侧魏制 ^置 下所示的化學式，使單結晶SlC成長：又件1中揭路有以如200811320 IX. Description of the invention: [Technical field to which the invention pertains] Materials for conductor elements or materials for LEDs are advantageous [Prior Art] Since single crystal SiC has a strong binding energy for crystallization, the dielectric field of insulation is large and the thermal conductivity is high, so It is quite effective as a component or power component for harsh environments. In addition, since its lattice constant is close to the crystal J constant of GaN, it is also used as a counter material for GaN-LED; there is a tradition that the production of such single crystal SiC includes: J SiC powder sublimation, on the inner wall of the graphite hanging 使 彡 彡 / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / / Improved riuri method for ^^ ΪΪίίί^θ; CVD method for epitaxial growth of a gas source by chemical reaction; and sublimation proximity method of fre crystal generated by graphite, ^sic^slCi Γ (Please refer to the non-patent grammar, S, 'the manufacturer of the various single-crystal SiC introduced above, quot; φ 疋 that still has its own problems. First, the self-made crystallinity is good in the disk. Single crystal sic, but because of this weighting method 状 = shape control and crystal surface control, one ^ ^ to a large number of high-speed formula into the dirty, lose the problem of 200811320. And in the CVD method, __ manufacturing high Purity and low defects, but because this manufacturing method is based on a thin gas source, The growth rate of the long crystal is slow, and the growth rate is 1Q/zm/h or less Βθ growth' The problem of the long single crystal SiC ingot cannot be obtained. Wang, and there is a sublimation approaching the towel, _ can be simple == 2: The method of reducing the cerium oxide by carbon on the carbon super-crystal on the structure. The seed is early, and the same. = ίί=ί^Γ. The high-quality single crystal of the product f is obtained at a high speed and owes to the bean 3 In the manufacturing method of the single crystal Sic disclosed in the above, the various methods of the apparatus such as the off-method, the supply of green, and the ring-shaped body; the structure of the apparatus such as the r method, and the chemical formula shown by the sub-wei system are Let the single crystal SlC grow up:

Sl〇2 + 3C — SiC + 2C〇 丨...化學式(1) 根據此化學式⑴的理想配比 耳的碳發生反應。 了^糾的-il切’ 3莫 f ί 日本麵第35G5597號公報 【非專利文件1】編著，「 日刊工業新聞社（2叫3月初版發行广體沉技術與應用」 【發明内容】 ^ΜΜΜΜ^ΜΜ 單結’倾供—種可長_，且穩定地使 θ 、為猫晶的改良方法；以及依據該方法而得到的高 200811320 σπ 質單結晶Sic。 解決謀題之丰與 2之課ί，可依據以下所記载的方式加以解決。 勺土明之單結晶SiC的製造方法，其特徵在於：、 slC ^用====的 以供應作為單結晶 _的步驟；以及， Μ)粒子之顧供應管，設置於相 料與tii ϊΐί境ΐ體Af掛_，將該單結晶sic製造用原 以使該單^===_供應__種結晶上，Sl〇2 + 3C — SiC + 2C〇 丨...chemical formula (1) According to the stoichiometric ratio of the chemical formula (1), the carbon of the ear reacts. ^ 的 的 - il cut ' 3 Mo f ί Japanese No. 35G5597 Bulletin [Non-Patent Document 1] edited, "Japan Industrial News Agency (2 called the first edition of the March issue of the wide body sink technology and application) [Summary] ^ ΜΜΜΜ^ΜΜ Single junction 'pour supply—the species can grow longer _, and θ is a modified method for cat crystals stably; and the high 200811320 σπ single crystal Sic obtained according to the method. The course ί can be solved according to the method described below. The method for producing the single crystal SiC of the present invention is characterized in that: slC ^ is used as the step of supplying the single crystal _ with ====; and, Μ) The particle supply tube is disposed on the phase material and the tii ϊΐ ΐ ΐ A , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , ,

= ^ΐ®'ί Sl°2 ： C 在化學式中以c表示。 Λ；> D，車父佳為石炭黑粒子’ 刻意==ΞΙί r⑽2及c之比， ——成比祕化，從岭成本ί:;?ί芯反，I，絲Οχ之組 ⑽2細_相對;;之 =£:介足 ^外，此輸歡地使單結 種方由的製造方法。而根據此 成比，藉由使如2的_比^^子所構成的原料的供應組 過剩供給时^，而獲得縣配比之城比更為 時間且敎猶造觀方式係可長 【實施方式】 200811320 就本發明所使用之單結晶Sic製 述莫耳比的範圍内，混合後的二氧切粒上 物。較佳的情況係可利用由粒徑整齊 子的此合 子所構成雜體粒子之混合物。又，此4^:^雜子及碳粒 麵、粒徑、粒子形狀等並無特別的=氧=粒子及雜子的 水解法（flame hydrolysis )所獲得之古 i如’可利用以火談 高純度乙炔黑（a_leneblacf)%之Γ純度—减以壎朴或 上者;及碳粒子中的任何一種’皆可用混合兩種以 行1广？ # 3」t可以視必要而對該二氧切粒子及碳粒子進 = = 添加其他成分皆可。將此等原料的比例設定 成在. C之莫耳比為Si〇2 : c=1〇5 : 3 〇〇〜2 〇〇 : \ 琴内而混合後，供應給種結晶。 .、靶 如上所遠，可將二氧化石夕藉由使其比理想配比更為 ^ ’。而得到邱良好的單結晶沉，此種結構可以如下的方式被推 ———…二奭認:為，在Sic進行成長之超過2〇〇(TC的高溫下，以上述 ^化學式(1)所表示白勺Si〇2在與C進行反應之前，其一部分會蒸 發。此=可從Si〇2的熔點（17〇〇π左右）與矽的熔點（14〇(^c左 右）推定而得。從此等之熔點可知，實際的尽應係以如下的方式 所進行。 s!02 s Si0x (液態）+Si〇y (氣態）个…化學式⑺= ^ΐ®'ί Sl°2 : C is represented by c in the chemical formula. Λ;> D, the father of the car is a charcoal black particle ' Deliberate == ΞΙ ί r (10) 2 and c ratio, —— into the ratio of secret, from the cost of ί:;? 芯 core anti, I, silk Οχ group (10) 2 fine _ Relative;; ==: In addition to the outside of the ^, this is a manufacturing method that makes a single knot. According to this ratio, by making the supply group of the raw materials composed of _ 比^^^2, the supply ratio of the county ratio is more time-consuming and the system is longer. BEST MODE FOR CARRYING OUT THE INVENTION 200811320 A dioxic pellet obtained after mixing in a range of a molar ratio of a single crystal Sic used in the present invention. Preferably, a mixture of the heteroparticles composed of the zygote having a uniform particle size can be utilized. In addition, the 4^:^ heterozygote and the carbon particle surface, the particle size, the particle shape, and the like have no special = oxygen = particle and miscellaneous hydrolysis obtained by the flame. High purity acetylene black (a_leneblacf)% purity - subtracted from the simple or the upper; and any of the carbon particles 'can be mixed with two to broaden? # 3"t can be added to the dioxin particles and carbon particles as necessary = = Add other ingredients. The ratio of the raw materials is set such that the molar ratio of C is Si〇2: c=1〇5: 3 〇〇~2 〇〇 : \ After mixing in the piano, the crystal is supplied. . As far as the target is concerned, the dioxide can be made more than ideal stoichiometry. And get a good single crystal sink of Qiu, this structure can be pushed in the following way ---... Two 奭 :: For, Sic grows more than 2 〇〇 (TC high temperature, with the above ^ chemical formula (1) The Si 〇 2 is evaporated before it reacts with C. This = can be estimated from the melting point of Si 〇 2 (about 17 〇〇 π) and the melting point of 矽 (14 〇 (^ c) From the melting points of these, it is known that the actual operation is carried out in the following manner: s! 02 s Si0x (liquid) + Si〇y (gaseous) ... chemical formula (7)

SlOx (液態）+ C — Sic + c〇个 …化學式(3)SlOx (liquid) + C — Sic + c〇 ...chemical formula (3)

SiOx與SiOy中的又與^可用〇〜2的值代入。此外，因為在 上述的化學式(2)及化學式⑶中，並非表示其處於平衡狀態，因此 在此省略表示各成分的k成之數字。根據此化學式，與C實際進 行反應的是SiOx (液態）。在反應的過程中，因為si〇2i一部分 ，依據上述的化學式而被抽出，因此根據上述曰本專利第35〇5597 说公報中之化學式(1)，使Si02與C之原料供應比為1 ·· 3的話， 用以形成SiC的Si份量就會不足，導致生長停滯，或是無法確保 200811320The value of SiOx and SiOy can be substituted with the value of 〇~2. Further, since the above chemical formula (2) and chemical formula (3) do not mean that they are in an equilibrium state, the number k of each component is omitted here. According to this chemical formula, SiOx (liquid) is actually reacted with C. In the course of the reaction, since a part of si〇2i is extracted according to the above chemical formula, the raw material supply ratio of SiO 2 and C is 1 according to the chemical formula (1) in the above-mentioned Japanese Patent No. 35〇5597. · 3, the amount of Si used to form SiC will be insufficient, resulting in stagnant growth, or unable to ensure 200811320

SiC的組成比，而導致多結晶的產生。 的方Γ鱼將ϊ t氧子與碳粒子供應到sic種單結晶晶圓上 =古可不間斷地連續供應的方法，然而’其 連續輸送粉體ΐ即可。但是，為了避免在該 結晶】1C製造裝置内部有氧的混入，因此較佳的 構其中所取代的細型隱-) 的供 結晶晶圓上混合後的狀態下被供應 I論事g = 原料’或是分別供應之後 Q.r H卜在單結晶％中進行摻雜（<1°Ρ_)時，可在該單姓曰 SlC衣以用原料中作為固體源而混合，或是在單处晶= -内的環競體中作為氣體源，混合該摻雜成分亦。可。狀衣置 當利ΐί 形狀而適當選擇。例如，可適 式瑞里法而得之結晶晶圓係將依改良 輪者。種結晶 注曰溫度並無特別的限制’可以根據所欲的單 了曰巧的大小、純、種轉而適t設定。較佳 二 定而得化〜24GG°C的範圍内，此溫度例如可從_外側的ϋ測 制、生ΐ本發明之單結曰曰日siC的製造方法中所使用的單έ士曰Sic之 Πί ’其結構並無特__。也就是說，曰的大 小、掛禍加熱方法、綱材質、原料供應方法、環境以:》 200811320 =成，力、溫度控制方法等，可以根據所欲的單結晶s ϋ:开:狀二f類、早結晶SiC製造用原料之種類與數量等適者 =擇而付。例如’溫度測定與溫度控制，可使用歷溫度控制^ 在丨，ΐ本^月所使用的掛禍之形狀，關於其外形並無特別的限 二U 所欲的單結晶SiC的大小與形狀而適當選擇。另外， 考慮到使用溫度的翻，該的材f較佳為石墨製。另 配人:結晶晶圓座之形狀並無特別的限制，可以The composition ratio of SiC leads to the generation of polycrystals. The square carp will supply 氧t and carbon particles to the sic single crystal wafer. The method can be continuously supplied continuously, however, it can continuously transport the powder mash. However, in order to avoid the incorporation of oxygen in the inside of the 1C manufacturing apparatus, it is preferable to use a fine structure in which the substituted thin crystals are replaced by a state in which the crystal wafer is mixed. Or, after being separately supplied, Qr Hb is doped in a single crystal % (<1°Ρ_), and may be mixed as a solid source in the single-site S1C coating raw material, or in a single crystal = - The doping component is also mixed as a gas source in the inner ring body. can. The shape is set as appropriate. For example, a crystalline wafer system that is suitable for the Swiss Riley method will be improved. There is no particular limitation on the temperature of the crystallization. The size can be set according to the size, purity, and rotation of the desired one. Preferably, it is within a range of 〜24 GG ° C, and the temperature can be, for example, from the 外侧 outside measurement system, and the single έ 曰 Sic used in the manufacturing method of the single knot si siC of the present invention. Π ί 'The structure is not special __. That is to say, the size of the crucible, the method of heating the crucible, the material of the material, the method of supplying the raw materials, and the environment are: "200811320 = into, force, temperature control method, etc., according to the desired single crystal s ϋ: open: shape two f Types and quantities of raw materials for early-crystallized SiC manufacturing, etc. For example, 'temperature measurement and temperature control, can use the temperature control ^ in the shape of the 挂 丨 ΐ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ Appropriate choice. Further, the material f is preferably made of graphite in consideration of the use of the temperature. Others: The shape of the crystal wafer holder is not particularly limited,

SlC的大小與形狀而適當選擇。'然而，考相 使用溫，的範圍，該基座的材質較佳為石墨製。 芩调 單結晶Sic製造用原料的原料供應管之形狀並益特 ，限^可以配合所欲的單結晶SlC之大小與形狀而適當選 円ΐίϊ使3溫ΐ的範圍，該供應管的材·佳為石墨製。 圖1係頌不用以製造本發明之單結晶Sic裝置的 冬 式剖面圖，在此係使用高頻感應加熱爐10為例說明。 心 .查水^的密閉腔室1 a，設置碳製的賴職2 =Omm，咼度l50mm) ’而在該水冷的 ^ 有高頻感應加熱線圈3。 j °又置 曰曰掛瑪2内部上方’貫穿插入有用以固持SiC種單砝 =曰一曰囫^的基座5。此基座5延伸到密閉掛塌2的内部，可‘ 圖不的旋轉機構’㈣基觸中心軸為旋轉細轉動。9 此外，在此基座5糊示_端，被舒—可 鳩咖（嫩向）蝴流：此外、， Α _^卜/在基座下端’固持SiC種單結晶晶圓的表面之法線方 Ϊ nH與該基座的·方向略平行起到最大傾斜45。角為止的 辄圍=由設定’以在種結晶4上使(Sic單結晶）成長 在_閉綱2内的麵，貫穿插入有用以供應單结曰成， 衣造用原料粉末粒子之原料供應f 6。且料供膽6係^伸設 200811320 置到該高親應加熱爐1G的賴，藉由閥8與8, f 複數之原料儲存槽7及7· ’以及可獨立調節流 里之h性攜载氣體A之供應源（未圖示）連接。 土本發明所特定的莫耳比的範圍之内，供應Si〇2粒子及c粒 t (N°.2〜6)’以及在上述莫耳比的範圍之外的混 =1·⑻：3.⑻之比較例1 (Ναι);以及該混合 ίΐΐί! .〇〇之比較例2 (Ν〇.7)中’製造SiC而比較檢 成長的型態。將Si〇2粒子與c粒子事先混合好之後，在 使為設定好的供應莫耳比之情況下，·—個儲存槽内供應 至該检閉糊内部亦可。又’亦可藉由將Sic>2粒子與C粒子充& Ϊ不槽中’然後調節來自於個別的儲存槽之相對供應、 Ϊ工ίΐΐίϊ供應管内之惰性攜載氣體中混合，而作為單結 曰曰SiC衣&用原料，連續供應到該密閉坩堝的内部。 ㈣盧’可藉由未圖示之真空排氣系統與壓力調節 ^此之夕I、it ’ ί外，亦具備未圖示之惰性氣體替換機構。 ，施例中’雖然是採用將原料供應管設置在 =的下方，㈣基座設置切_上方之型態，但是在不改變 作ϊ的範圍内’亦可變更為與此上下相反的型態而設 ^此外，亦可使供應管姉於基座，呈斜喊橫向設置皆無不 【實施例】 ，用，頻感應加熱爐’依以下的條件，製造單結晶sic。於 以基座下端’固定SiC種單結晶晶圓。在此所使 i 、 晶晶圓、，，使用依改良式瑞里法所製的單結晶=S1C種早、、、。 作，单結晶Sic製造用原料的碳與Si〇2，分學 公司所生產魏f MA6G0以及日本Ae減公司生】予 ΓΛί抽取高頻感應加熱爐内部的空氣使之成為直空之後，以产 猎由該義感應加熱義，_韻的賴 二 11 200811320 5亥SiC種單結晶晶圓的表面溫度達到μ⑽。〇〜％⑻。〇的範圍 其次，將其上有SiC種單結晶晶圓固定之該基座，以0〜2〇rpm 旋轉速度使其旋轉。在此狀態下，調整成使該惰性攜载氣體（高 純度j氬）在流速a5L/min〜10L/min的範圍内使其流動。然^ • 將该單結晶Sic製造用原料，經由該供應管内部，使其連續供應 • 到設置於該密閉坩堝内的頂部之該SiC種單結晶晶圓的表^上了 以製造單結晶SiC。製造的結果歸納顯示於表！。 〔表1〕The size and shape of the SlC are appropriately selected. 'However, the temperature of the test is used, and the material of the base is preferably made of graphite.芩 芩 芩 结晶 结晶 S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S S Good for graphite. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a winter sectional view of a single crystal Sic apparatus which is not used in the manufacture of the present invention, and the high frequency induction heating furnace 10 is used as an example. Heart. Check the water's closed chamber 1 a, set the carbon-made Lai 2 = Omm, the twist is l50mm) and the water-cooled ^ has the high-frequency induction heating coil 3. The j ° is placed on the inside of the 玛 2 2, and the susceptor 5 which is used to hold the SiC species 砝 曰 曰囫 曰囫 。 is inserted. The susceptor 5 extends to the inside of the airtight sag 2, and can be rotated by a rotation of the center axis of the "rotation mechanism" (four). 9 In addition, the pedestal 5 is spliced at the _ end, and is smothered by the squeezing scent: in addition, Α _ ^ 卜 / at the lower end of the pedestal 'holding the surface of the SiC single crystal wafer The line square Ϊ nH is slightly parallel to the direction of the base to have a maximum inclination 45.辄 = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = f 6. And the material for the 6-series system is set to the high-response heating furnace 1G, with the valves 8 and 8, f multiple raw material storage tanks 7 and 7 · ' and can independently adjust the flow of h-carrying A supply source (not shown) of the carrier gas A is connected. Within the range of the specific molar ratio of the present invention, the Si 〇 2 particles and the c particles t (N°. 2 to 6)' and the mixture outside the range of the above molar ratio = 1 (8): 3 are supplied. (8) Comparative Example 1 (Ναι); and Comparative Example 2 (Ν〇.7) in which the SiC was produced and compared with the growth type. After the Si 〇 2 particles and the c particles are mixed in advance, when the supplied molar ratio is set, the storage tank may be supplied to the inside of the inspection paste. In addition, it can also be mixed by mixing the Sic>2 particles and the C particles with the C-particles and then adjusting the relative supply from the individual storage tanks and the inert carrier gas in the supply pipe. The crucible SiC coat & raw material is continuously supplied to the inside of the closed crucible. (4) Lu's vacuum exhaust system and pressure adjustment (not shown). In addition to the I, it's ί, there is also an inert gas replacement mechanism (not shown). In the example, although the raw material supply pipe is set below the =, (4) the pedestal is set to the upper y-type, but it can be changed to the opposite type without changing the ϊ. In addition, it is also possible to make the supply tube smashed on the pedestal, and it is arranged in a horizontal direction. [Example], a frequency induction heating furnace is used to manufacture a single crystal sic according to the following conditions. The SiC seed single crystal wafer is fixed at the lower end of the susceptor. Here, i, the crystal wafer, and the single crystal = S1C produced by the modified Rayleigh method are used. As a raw material for the production of single-crystal Sic, carbon and Si〇2, Wei f MA6G0 produced by Seiko Co., Ltd., and Ae Reduction Co., Ltd. of Japan] are extracted from the air inside the high-frequency induction heating furnace to make it into a straight space. Hunting by the sense of induction heating, _ rhyme of Lai 2 11 200811320 5 SiC SiC single crystal wafer surface temperature reached μ (10). 〇~%(8). The range of 〇 Next, the susceptor on which the SiC single crystal wafer is fixed is rotated at a rotation speed of 0 to 2 rpm. In this state, the inert carrier gas (high purity j argon) was adjusted to flow in a flow rate range of a5 L/min to 10 L/min. Then, the raw material for manufacturing the single crystal Sic is continuously supplied through the inside of the supply tube to the surface of the SiC single crystal wafer disposed on the top of the sealed crucible to manufacture single crystal SiC. . The results of the manufacturing are summarized in the table! . 〔Table 1〕

No. Si02 : C (莫耳比） 對成長膜之觀察結果 1 (比較例1) 1.00 ·· 3.00 在成長途中產生多结黑 2 (實施例1) 1.05 ： 3.00 —----—--- ^ 、、、口曰日 早結晶成長 3 (實施例2) 1.25 ： 3.00 早結晶成長 4 (實施例3 ) 1.50 ： 3.00 單結晶成長 5 (實施例4) 1.75 : 3.00 單結晶成；§___ 早結晶成‘___ 成長速度極端降低 胃6_ (實施例 7 (比較例2) 2.00 : 3.00 —------- 2.10 ： 3.00No. Si02 : C (Morby) Observation result of the grown film 1 (Comparative Example 1) 1.00 ·· 3.00 Multi-junction black was generated during growth (Example 1) 1.05 : 3.00 —------- - ^ , , , 口 口 early day crystal growth 3 (Example 2) 1.25 : 3.00 Early crystal growth 4 (Example 3) 1.50 : 3.00 Single crystal growth 5 (Example 4) 1.75 : 3.00 Single crystal formation; §___ Early crystallization into '___ growth rate extremely lower stomach 6_ (Example 7 (Comparative Example 2) 2.00: 3.00 —------- 2.10 : 3.00

如表1所示，在將Si02 : c (莫耳比）設於1〇5 : 3 〇〜 3.0的範圍内供應時，可使單結晶Si(：穩定地成長。 . 12 200811320 【圖式簡單說明】 _ 圖1係顯示用以製造本發明之單結晶Sic裝置的一例之概念 式剖面圖。 【主要元件符號說明】 1〜密閉腔室 2〜密閉坩堝 3〜高頻感應加熱線圈 4〜SiC種單結晶晶圓（種結晶） 5〜基座 6〜原料供應管 7、 7’〜原料儲存槽 8、 8’〜調節閥 9〜（SiC單結晶）成長層 10〜高頻感應加熱爐 A〜惰性攜載氣體As shown in Table 1, when SiO 2 : c (mole ratio) is supplied in the range of 1 〇 5 : 3 〇 to 3.0, single crystal Si can be grown (steadily grown. 12 200811320 [Simple diagram BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a conceptual cross-sectional view showing an example of a single crystal Sic device for manufacturing the present invention. [Description of main components] 1 to a closed chamber 2 to a closed 〜3 to a high frequency induction heating coil 4 to SiC Single crystal wafer (species crystal) 5~ pedestal 6~ raw material supply pipe 7, 7'~ raw material storage tank 8, 8'~ regulating valve 9~ (SiC single crystal) growing layer 10~ high frequency induction heating furnace A ~Inert carrier gas

1313

Claims (1)

200811320 十、申請專利範圍·· 1. 一種早結晶SiC的髮造方法，其特徵在於： 包含： 將固定有SiC種結晶的基座；與用以供應作為單έ士曰制 g原^的Sl〇2粒子及碳(C)粒子之原料供應f，設置堝‘ 在具有高溫環境氣體之該坩堝内，將該單結晶 料與惰性觀㈣-起，軸該補供細編曰用原 以使該單結晶Sic成長的步驟； 禋'、、^日上， C—ϋ，作f原料的呢與c之供應莫耳比的範圍為Si〇2 : 。一 1·05 · 3.0〜2.0 : 3.0 〇 該.^第1項之單結晶sic的製造方法，其中， 晶_糊娜1或2項之單結 十一、圖式·· 14200811320 X. Patent Application Scope 1. A method for producing early-crystallized SiC, comprising: a susceptor to which SiC crystals are immobilized; and Sl for supplying g as a single gentleman The raw material supply f of the 〇2 particles and the carbon (C) particles is set to 埚' in the crucible having a high-temperature ambient gas, and the single crystal material is mixed with the inertia (four), and the shaft is supplemented with the original The step of growing the single crystal Sic; 禋', , ^, C, ϋ, the ratio of the supply of the raw material to the molar ratio of c is Si〇2 : . A 1.05 · 3.0~2.0 : 3.0 〇 The manufacturing method of the single crystal sic of the first item, ^, the single knot of the crystal 1 or 2, XI, Fig. 14
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