JP2000001398A - Production of silicon carbide semiconductor substrate - Google Patents
Production of silicon carbide semiconductor substrateInfo
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- JP2000001398A JP2000001398A JP16033898A JP16033898A JP2000001398A JP 2000001398 A JP2000001398 A JP 2000001398A JP 16033898 A JP16033898 A JP 16033898A JP 16033898 A JP16033898 A JP 16033898A JP 2000001398 A JP2000001398 A JP 2000001398A
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- Prior art keywords
- silicon carbide
- hydrogen chloride
- sic
- face
- semiconductor substrate
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- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、半導体素子を形成
する炭化けい素基板の製造方法に関する。The present invention relates to a method for manufacturing a silicon carbide substrate for forming a semiconductor device.
【０００２】[0002]
【従来技術】高周波、大電力の制御を目的として、シリ
コン（以下Ｓｉと記す）を用いた電力用半導体素子（以
下パワーデバイスと称する）では、各種の工夫により高
性能化が進められている。しかし、パワーデバイスは高
温や放射線等の存在下で使用されることもあり、そのよ
うな条件下ではＳｉのパワーデバイスは使用できないこ
とがある。2. Description of the Related Art For the purpose of controlling high frequency and large power, a power semiconductor device (hereinafter, referred to as a power device) using silicon (hereinafter, referred to as Si) has been improved in performance by various means. However, the power device may be used in the presence of high temperature or radiation, and under such conditions, the Si power device may not be used.
【０００３】また、Ｓｉのパワーデバイスより更に高性
能のものを求める声に対して、新しい材料の適用が検討
されている。本発明でとりあげる炭化けい素（以下Ｓｉ
Ｃと記す）は広い禁制帯幅（４Ｈ−ＳｉＣで３．２６ｅ
Ｖ、６Ｈ−ＳｉＣで３．０２ｅＶ）をもつため、高温で
の電気伝導度の制御性や耐放射線性に優れ、またＳｉよ
り約１桁高い絶縁破壊電圧をもつため、高耐圧素子への
適用が可能である。さらに、ＳｉＣはＳｉの約２倍の電
子飽和ドリフト速度をもつので、高周波大電力制御にも
適する。Further, in response to a demand for a device having a higher performance than a Si power device, application of a new material is being studied. Silicon carbide (hereinafter referred to as Si)
C has a wide band gap (3.26e for 4H-SiC)
V, 3.02 eV in 6H-SiC), so it is excellent in controllability of electric conductivity at high temperature and radiation resistance, and it has a breakdown voltage about one digit higher than that of Si, so it can be applied to high breakdown voltage devices. Is possible. Further, since SiC has an electron saturation drift speed about twice as high as that of Si, it is also suitable for high frequency high power control.
【０００４】しかし、ＳｉＣの優れた物性をパワーデバ
イスに応用するためには、Ｓｉのプロセス技術並みに洗
練された要素技術が必要となる。すなわち、ＳｉＣ基板
の表面を鏡面に仕上げた後、ＳｉＣ薄膜をエピタキシャ
ル成長させ、或いはドナーやアクセプターをドーピング
したり、金属膜や酸化膜を形成する等の工程条件の最適
化が必要である。[0004] However, in order to apply the excellent physical properties of SiC to a power device, element technology as sophisticated as Si process technology is required. That is, after the surface of the SiC substrate is mirror-finished, it is necessary to optimize process conditions such as epitaxially growing a SiC thin film, doping a donor or an acceptor, or forming a metal film or an oxide film.
【０００５】エピタキシャル成長においては、意図した
キャリア密度をもち、かつ結晶性のよい薄膜を得ること
が重要である。従来、ＳｉＣのエピタキシャル成長は、
モノシラン、プロパンを反応ガスとして、約１５００℃
でおこなわれていた。従来、Ｓｉのエピタキシャル成長
においては、原料ガスに塩素を含むシランガス（例えば
ＳｉＣｌ4 ）を用いることは知られていた。これに対
し、ＳｉＣ上のエピタキシャル成長においては、立方晶
の３Ｃ−ＳｉＣを成膜する原料ガスとしてＳｉＣｌ2 Ｈ
2 等を用いた報告［例えば、E.niemann et al. Inst. P
hys. Conf. Ser. No.142, pp.165-168 参照］や、シリ
コンサブストレート上への３Ｃ−ＳｉＣのヘテロエピタ
キシャル成長のために塩素を含む炭化水素（例えばＣＨ
3Ｃｌ）を用いる出願［特開平４−１２４８１５号］が
あるだけで、六方晶の４Ｈまたは６Ｈ−ＳｉＣの薄膜成
長についてはそのような例もなく、塩化水素を添加する
ことは知られていなかった。[0005] In epitaxial growth, it is important to obtain a thin film having an intended carrier density and good crystallinity. Conventionally, epitaxial growth of SiC has
About 1500 ° C using monosilane and propane as reaction gases
It was done in. Conventionally, it has been known to use a silane gas containing chlorine (eg, SiCl 4 ) as a source gas in epitaxial growth of Si. On the other hand, in epitaxial growth on SiC, SiCl 2 H is used as a source gas for forming a cubic 3C—SiC film.
Report using 2 etc. [For example, E.niemann et al. Inst.
hys. Conf. Ser. No. 142, pp. 165-168], and hydrocarbons containing chlorine (for example, CH 3 for heteroepitaxial growth of 3C—SiC on a silicon substrate).
There is only an application using [ 3 Cl) [Japanese Patent Application Laid-Open No. 4-124815], and there is no such example of the growth of a hexagonal 4H or 6H-SiC thin film, and it is not known to add hydrogen chloride. Was.
【０００６】また、六方晶の４Ｈまたは６Ｈ−ＳｉＣの
薄膜成長に関して、薄膜成長前の基板の表面処理に塩化
水素を用いた例がある［例えば、A.A.Burk,Jr., L.B.Ro
wland, J. Crystal Growth, vol.167, pp.586-595,(199
6)参照］。この処理により成長層表面のモホロジーが制
御できるとされている。また同様の基板処理により基板
／成長層界面のアルミの意図しないドーピングを抑制で
きることが報告されている［A.A.Burk,Jr., L.B.Rowlan
d, Appl.Phys.Lett, vol.68, pp.382-384 1996. ］。As for the growth of hexagonal 4H or 6H-SiC thin films, there is an example in which hydrogen chloride is used for the surface treatment of a substrate before the growth of the thin film [for example, AA Burk, Jr., LBRo.
wland, J. Crystal Growth, vol.167, pp.586-595, (199
6)]. It is said that the morphology of the growth layer surface can be controlled by this treatment. It has also been reported that similar substrate treatment can suppress unintended doping of aluminum at the substrate / growth layer interface [AABurk, Jr., LB Rowlan
d, Appl. Phys. Lett, vol. 68, pp. 382-384 1996.].
【０００７】[0007]
【発明が解決しようとする課題】優れた特性のＳｉＣ半
導体素子とするためには、ＳｉＣ薄膜のエピタキシャル
成長においても、一層良質のエピタキシャル層すなわ
ち、意図したキャリア密度をもち、かつ結晶欠陥密度が
低く結晶性のよい薄膜を得ることが課題である。In order to obtain a SiC semiconductor device having excellent characteristics, even in the epitaxial growth of a SiC thin film, an epitaxial layer of higher quality, that is, a crystal having an intended carrier density and a low crystal defect density, is required. The challenge is to obtain a good thin film.
【０００８】[0008]
【課題を解決するための手段】発明者はエピタキシャル
成長時に塩化水素を添加する実験をおこなった結果、塩
化水素添加が有効であることを見いだした。上記課題解
決のため本発明は、炭化けい素基板上に炭化けい素エピ
タキシャル層を成長させる炭化けい素半導体基板の製造
方法において、塩化水素を添加した雰囲気中でエピタキ
シャル層を成長するものとする。The inventor conducted an experiment in which hydrogen chloride was added during epitaxial growth, and found that hydrogen chloride addition was effective. To solve the above problems, the present invention provides a method for manufacturing a silicon carbide semiconductor substrate in which a silicon carbide epitaxial layer is grown on a silicon carbide substrate, wherein the epitaxial layer is grown in an atmosphere containing hydrogen chloride.
【０００９】そのようにすれば、基板表面の清浄化がお
こなわれ、結晶欠陥であるエッチピット密度が減少し、
例えば、キャリア移動度などエピタキシャル層の膜質が
向上する。特に、塩化水素の添加量を体積比で０．１〜
０．８％、更に望ましくは０．２〜０．６％とするのが
よい。By doing so, the surface of the substrate is cleaned, the density of etch pits as crystal defects is reduced,
For example, the film quality of the epitaxial layer such as carrier mobility is improved. In particular, the addition amount of hydrogen chloride is 0.1 to
0.8%, more preferably 0.2 to 0.6%.
【００１０】０．２〜０．６％の濃度範囲においては、
一層効果が顕著になる。炭化けい素サブストレートが、
４Ｈ−ＳｉＣまたは６Ｈ−ＳｉＣであるものとする。４
Ｈ−ＳｉＣまたは６Ｈ−ＳｉＣは、広い禁制帯幅を有す
る高温用半導体素子等に適する結晶であり、実施例に示
したように塩化水素ガスの添加により、結晶性の改善が
見られた。In the concentration range of 0.2 to 0.6%,
The effect becomes more remarkable. Silicon carbide substrate
It is assumed to be 4H-SiC or 6H-SiC. 4
H-SiC or 6H-SiC is a crystal suitable for a high-temperature semiconductor device or the like having a wide forbidden band width. As shown in Examples, the addition of hydrogen chloride gas has improved the crystallinity.
【００１１】炭化けい素サブストレートの表面は（００
０１）Ｓｉ面、（０００−１）炭素面またはそれらの面
から数度のオフセット角を持つ面であるものとする。そ
のような結晶面は、平滑な面が得られ、エピタキシャル
成長に適する面である。The surface of the silicon carbide substrate is (00
01) Si plane, (000-1) carbon plane, or a plane having an offset angle of several degrees from those planes. Such a crystal plane has a smooth surface and is suitable for epitaxial growth.
【００１２】[0012]
【発明の実施の形態】以下本発明のためにおこなった実
験および実施例について説明する。 ［実験１］エピタキシャル成長前のサブストレート（以
下基板と呼ぶ）としては鏡面研磨された４Ｈ−ＳｉＣ単
結晶を用い、（０００１）Ｓｉ面から〈１、１、−２、
０〉方向に８度傾けて研磨した面を使用した。DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, experiments and examples performed for the present invention will be described. [Experiment 1] A mirror-polished 4H—SiC single crystal was used as a substrate (hereinafter referred to as a substrate) before epitaxial growth, and a <1,1, −2,
A surface polished at an angle of 8 degrees in the 0> direction was used.
【００１３】先ず、基板をダイサーにより５ｍｍ角のチ
ップに切り分け、有機溶剤と酸による洗浄をした後、エ
ッチングするＳｉ面を上にして、基板をＳｉＣで被覆し
た黒鉛のサセプタに載せる。基板を載せたサセプタを石
英反応管内に挿入し、１Ｐａ以下の真空にひく。次に気
相エッチングをおこなう。気相エッチングは、水素と塩
化水素をそれぞれ毎分１Ｌ、１０ｍＬの流量で混ぜた混
合ガスを流しながら１３５０℃で５分間加熱した。サセ
プタの加熱法は高周波誘導加熱である。First, the substrate is cut into 5 mm square chips by a dicer, washed with an organic solvent and an acid, and placed on a graphite susceptor coated with SiC with the Si surface to be etched facing up. The susceptor on which the substrate is placed is inserted into a quartz reaction tube, and a vacuum of 1 Pa or less is applied. Next, vapor phase etching is performed. In the gas phase etching, heating was performed at 1350 ° C. for 5 minutes while flowing a mixed gas obtained by mixing hydrogen and hydrogen chloride at a flow rate of 1 L / min and 10 mL / min. The method of heating the susceptor is high-frequency induction heating.
【００１４】続いてＳｉＣ薄膜をエピタキシャル成長す
る。水素（Ｈ2 ）、モノシラン（ＳｉＨ4 ）、プロパン
（Ｃ3 Ｈ8 ）、塩化水素（ＨＣｌ）をそれぞれ毎分３
Ｌ、０．３ｍＬ、０．２５ｍＬ、３〜３０ｍＬの流量比
率で混合したものを反応管内に導入した。この状態で１
５００℃で２時間加熱した。すると基板上に４Ｈ型のＳ
ｉＣ薄膜がエピタキシャル成長する。薄膜のキャリア密
度は５×１０15ｃｍ-3であった。Subsequently, a SiC thin film is epitaxially grown. Hydrogen (H 2 ), monosilane (SiH 4 ), propane (C 3 H 8 ), and hydrogen chloride (HCl) were added at a rate of 3 minutes per minute.
A mixture of L, 0.3 mL, 0.25 mL, and a flow rate of 3 to 30 mL was introduced into the reaction tube. In this state, 1
Heated at 500 ° C. for 2 hours. Then, 4H-type S on the substrate
An iC thin film grows epitaxially. The carrier density of the thin film was 5 × 10 15 cm −3 .
【００１５】成長した膜の転位密度を評価するために、
水酸化カリウム（ＫＯＨ）によるエッチングをおこなっ
た。このエッチングは、ニッケル（Ｎｉ）坩堝内で４０
０℃に加熱した水酸化カリウムに試料を３０秒間浸漬す
る方法を用いた。欠陥密度の計数はＳＥＭ観察によっ
た。図１は、エピタキシャル成長時の塩化水素濃度［Ｈ
Ｃｌ／（Ｈ2 ＋ＳｉＨ4 ＋Ｃ3 Ｈ8 ＋ＨＣｌ）］とＳｉ
Ｃ薄膜中のエッチピット密度との関係を示す特性図であ
る。この図から塩化水素濃度が０．１から０．８％でエ
ッチピット密度が減少し、特に０．２から０．６％のと
き、顕著に減少し塩化水素を添加しない場合より約一桁
低減できることがわかる。In order to evaluate the dislocation density of the grown film,
Etching with potassium hydroxide (KOH) was performed. This etching is performed in a nickel (Ni) crucible at 40
A method of immersing the sample in potassium hydroxide heated to 0 ° C. for 30 seconds was used. Defect density was counted by SEM observation. FIG. 1 shows the concentration of hydrogen chloride [H
Cl / (H 2 + SiH 4 + C 3 H 8 + HCl)] and Si
FIG. 4 is a characteristic diagram showing a relationship with an etch pit density in a C thin film. From this figure, it can be seen that the etch pit density decreases when the hydrogen chloride concentration is 0.1 to 0.8%, especially when the hydrogen chloride concentration is 0.2 to 0.6%, and is reduced by about one digit compared to the case where no hydrogen chloride is added. We can see that we can do it.
【００１６】エッチピットは、エピタキシャル層中の線
状欠陥である転位の位置にできるのであり、結晶性の良
否を反映するともに、電気的にはキャリアのトラップに
なるとされている。図２は、発明者らが実験したエッチ
ピット密度とキャリアの移動度との関係を示す特性図で
ある。エッチピット密度が多いほど、移動度が急速に低
下している。これから、エッチピット密度を一桁減らせ
ば、移動度をほぼ２倍にできることがわかる。なお、移
動度の評価法としては、van der Pauw 法を用いた。す
なわち、試料のエピタキシャル層上の四隅に、金属マス
クを使ったスパッタ法によりニッケル（Ｎｉ）電極を形
成する。電極の直径は２００μｍ、厚さは４００ｎｍで
ある。この後、整流性を除きオーミックな接触とするた
めアルゴン（Ａｒ）雰囲気中で１０５０℃、５分間のア
ニールをおこなった。The etch pits can be formed at the positions of dislocations, which are linear defects in the epitaxial layer. The etch pits reflect the quality of crystallinity and are considered to electrically trap carriers. FIG. 2 is a characteristic diagram showing the relationship between the etch pit density and the mobility of carriers, which were experimented by the inventors. As the etch pit density increases, the mobility decreases rapidly. This shows that the mobility can be almost doubled by reducing the etch pit density by one digit. The mobility was evaluated by the van der Pauw method. That is, nickel (Ni) electrodes are formed at four corners on the epitaxial layer of the sample by a sputtering method using a metal mask. The diameter of the electrode is 200 μm and the thickness is 400 nm. Thereafter, annealing was performed at 1050 ° C. for 5 minutes in an argon (Ar) atmosphere to obtain ohmic contact without rectification.
【００１７】従って、図１、２から、成長するエピタキ
シャル層の結晶性は、塩化水素濃度が０．１〜０．８
％、更に望ましくは０．２〜０．６％含まれるとき改善
されるので、そのような条件でエピタキシャル成長をお
こなうのが良いと結論づけられる。これは、エピタキシ
ャル成長時に、表面の清浄化およびエッチングが十分に
行われるためと考えられる。また、シリコン半導体にお
いて見られる金属不純物のゲッタリング作用もあるかも
しれない。Therefore, from FIGS. 1 and 2, the crystallinity of the epitaxial layer to be grown is determined when the hydrogen chloride concentration is 0.1 to 0.8.
%, More preferably 0.2-0.6%, it is concluded that it is better to perform epitaxial growth under such conditions. This is presumably because the surface is sufficiently cleaned and etched during the epitaxial growth. There may also be a gettering effect of metal impurities found in silicon semiconductors.
【００１８】上記実施例では１５００℃のエッチング条
件における結果のみを記したが、１４５０から１５５０
℃の範囲において同様の実験をおこない、１４５０℃で
は塩化水素濃度を０．５〜１％、１５５０℃では濃度を
０．１〜０．３％とするとよいことがわかった。また成
長面についても４Ｈ−ＳｉＣの（０００１）Ｓｉ面だけ
でなく、４Ｈ−ＳｉＣの（０００−１）Ｃ面や６Ｈ−Ｓ
ｉＣのＳｉ、Ｃ面、またはそれらの面から微小角度で傾
斜した面にも適用できる。In the above embodiment, only the result under the etching condition of 1500 ° C. is described.
A similar experiment was conducted in the range of ° C, and it was found that the hydrogen chloride concentration at 1450 ° C should be 0.5 to 1%, and the concentration at 1550 ° C should be 0.1 to 0.3%. The growth surface is not only the (0001) Si plane of 4H-SiC, but also the (000-1) C plane of 4H-SiC or 6H-S
The present invention can also be applied to a Si or C plane of iC or a plane inclined at a small angle from those planes.
【００１９】[0019]
【発明の効果】以上説明したように本発明によれば、Ｓ
ｉＣ半導体基板のエピタキシャル成長時に、体積比で
０．１〜１．０％の塩化水素を添加し、１４５０〜１５
５０℃で成長することによって、成長するエピタキシャ
ル層の結晶性を改善し、ＳｉＣ半導体素子の特性を向上
させることができる。As described above, according to the present invention, S
During epitaxial growth of the iC semiconductor substrate, hydrogen chloride of 0.1 to 1.0% by volume is added, and 1450 to 15% is added.
By growing at 50 ° C., the crystallinity of the grown epitaxial layer can be improved, and the characteristics of the SiC semiconductor device can be improved.
【図１】エピタキシャル成長時ＨＣｌ濃度とエッチピッ
ト密度の関係を示す特性図FIG. 1 is a characteristic diagram showing a relationship between HCl concentration and etch pit density during epitaxial growth.
【図２】エッチピット密度と移動度との関係を示す特性
図FIG. 2 is a characteristic diagram showing a relationship between etch pit density and mobility.
Claims (5)
ャル層を成長させる炭化けい素半導体基板の製造方法に
おいて、塩化水素ガスを添加した雰囲気中でエピタキシ
ャル層を成長することを特徴とする炭化けい素半導体基
板の製造方法。1. A method for manufacturing a silicon carbide semiconductor substrate, comprising the steps of: growing a silicon carbide epitaxial layer on a silicon carbide substrate, wherein the epitaxial layer is grown in an atmosphere to which hydrogen chloride gas is added. Manufacturing method of elementary semiconductor substrate.
とすることを特徴とする請求項１記載の炭化けい素半導
体基板の製造方法。2. The addition amount of hydrogen chloride is 0.1 to 1% by volume.
2. The method for manufacturing a silicon carbide semiconductor substrate according to claim 1, wherein:
６％とすることを特徴とする請求項１記載の炭化けい素
半導体基板の製造方法。3. The amount of hydrogen chloride to be added is 0.2 to 0.1 in volume ratio.
2. The method for producing a silicon carbide semiconductor substrate according to claim 1, wherein the content is 6%.
Ｃまたは６Ｈ−ＳｉＣであることを特徴とする請求項１
ないし３のいずれかに記載の炭化けい素半導体基板の製
造方法。4. The method according to claim 1, wherein the silicon carbide substrate is 4H-Si.
C or 6H-SiC.
4. The method for manufacturing a silicon carbide semiconductor substrate according to any one of items 1 to 3.
０１）Ｓｉ面、（０００−１）炭素面またはそれらの面
から数度のオフセット角を持つ面であることを特徴とす
る請求項４記載の炭化けい素半導体基板の製造方法。5. The method of claim 1, wherein the surface of the silicon carbide substrate is (00).
5. The method for manufacturing a silicon carbide semiconductor substrate according to claim 3, wherein the surface is a (01) Si surface, a (000-1) carbon surface, or a surface having an offset angle of several degrees from those surfaces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16033898A JP3915252B2 (en) | 1998-06-09 | 1998-06-09 | Method for manufacturing silicon carbide semiconductor substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| JP16033898A JP3915252B2 (en) | 1998-06-09 | 1998-06-09 | Method for manufacturing silicon carbide semiconductor substrate |
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| JP2000001398A true JP2000001398A (en) | 2000-01-07 |
| JP3915252B2 JP3915252B2 (en) | 2007-05-16 |
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| WO2005055323A1 (en) * | 2003-12-03 | 2005-06-16 | The Kansai Electric Power Co., Inc. | Silicon carbide semiconductor device and its manufacturing method |
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