JP6996425B2 - Method for fixing raw material crystal rods, method for manufacturing semiconductor single crystals, and packaging materials for raw material crystal rods - Google Patents

Method for fixing raw material crystal rods, method for manufacturing semiconductor single crystals, and packaging materials for raw material crystal rods Download PDF

Info

Publication number
JP6996425B2
JP6996425B2 JP2018105046A JP2018105046A JP6996425B2 JP 6996425 B2 JP6996425 B2 JP 6996425B2 JP 2018105046 A JP2018105046 A JP 2018105046A JP 2018105046 A JP2018105046 A JP 2018105046A JP 6996425 B2 JP6996425 B2 JP 6996425B2
Authority
JP
Japan
Prior art keywords
raw material
crystal rod
material crystal
packaging material
fixing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
JP2018105046A
Other languages
Japanese (ja)
Other versions
JP2019210163A (en
Inventor
直樹 永井
聡 鈴木
義博 児玉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shin Etsu Handotai Co Ltd
Original Assignee
Shin Etsu Handotai Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shin Etsu Handotai Co Ltd filed Critical Shin Etsu Handotai Co Ltd
Priority to JP2018105046A priority Critical patent/JP6996425B2/en
Publication of JP2019210163A publication Critical patent/JP2019210163A/en
Application granted granted Critical
Publication of JP6996425B2 publication Critical patent/JP6996425B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Crystals, And After-Treatments Of Crystals (AREA)

Description

本発明は、ＦＺ法による半導体単結晶の製造に関する。 The present invention relates to the production of a semiconductor single crystal by the FZ method.

シリコン単結晶を製造する方法として、ＦＺ法が知られている。従来、高耐圧パワーデバイスやサイリスタ等のパワーデバイス製造用には、ＦＺ法により製造された高純度シリコンウェーハが使用されてきた。近年では、半導体デバイスの性能向上とコストの低減のため、大口径のシリコンウェーハが求められ、これに伴って大口径シリコン単結晶の育成が要求されている（特許文献１参照）。 The FZ method is known as a method for producing a silicon single crystal. Conventionally, high-purity silicon wafers manufactured by the FZ method have been used for manufacturing power devices such as high-voltage power devices and thyristors. In recent years, in order to improve the performance of semiconductor devices and reduce costs, silicon wafers having a large diameter have been required, and along with this, the growth of large-diameter silicon single crystals has been required (see Patent Document 1).

図１に、一般的に用いられるＦＺ単結晶製造装置３０を示す。
このＦＺ単結晶製造装置３０を用いて、シリコン単結晶を製造する方法について説明する。原料結晶棒１をチャンバー２０内に設置された上軸３の上部保持治具４に保持させ、直径の小さい種結晶（単結晶の種）８を、原料結晶棒１の下方に位置する下軸５の下部保持治具６に保持させる。次に、誘導加熱コイル７により原料結晶棒１を溶融して、種結晶８に融着させる。その後、種絞りにより絞り部９を形成して無転位化する。そして、上軸３と下軸５とを回転させながら、原料結晶棒１とシリコン単結晶である単結晶棒２とを下降させることで浮遊帯域（溶融帯あるいはメルトともいう）１０を原料結晶棒１と単結晶棒２の間に形成し、当該浮遊帯域１０を原料結晶棒１の上端まで移動させてゾーニングし、単結晶棒２を成長させる。この成長は、Ａｒガスに微量の窒素ガスを混合した雰囲気中で行われる。なお、上記誘導加熱コイル７としては、銅または銀からなる単巻または複巻の冷却用の水を流通させた誘導加熱コイルが用いられている。 FIG. 1 shows a commonly used FZ single crystal manufacturing apparatus 30.
A method of manufacturing a silicon single crystal using this FZ single crystal manufacturing apparatus 30 will be described. The raw material crystal rod 1 is held by the upper holding jig 4 of the upper shaft 3 installed in the chamber 20, and the seed crystal (single crystal seed) 8 having a small diameter is placed on the lower shaft located below the raw material crystal rod 1. It is held by the lower holding jig 6 of 5. Next, the raw material crystal rod 1 is melted by the induction heating coil 7 and fused to the seed crystal 8. After that, the drawing portion 9 is formed by a seed drawing to make the drawing portion non-dislocation. Then, while rotating the upper shaft 3 and the lower shaft 5, the raw material crystal rod 1 and the single crystal rod 2 which is a silicon single crystal are lowered to create a floating zone (also referred to as a melt zone or a melt) 10 as a raw material crystal rod. It is formed between 1 and the single crystal rod 2, and the floating zone 10 is moved to the upper end of the raw material crystal rod 1 for zoning to grow the single crystal rod 2. This growth is carried out in an atmosphere in which a trace amount of nitrogen gas is mixed with Ar gas. As the induction heating coil 7, an induction heating coil in which single-wound or double-wound cooling water made of copper or silver is circulated is used.

特開２０１０－１３２４７０号公報Japanese Unexamined Patent Publication No. 2010-132470

通常、原料結晶棒１は、上軸３の上部保持治具４にて保持する必要があるため、原料結晶棒１の上側（単結晶になった時のテール側）を予め機械加工したり、下側（単結晶になった時のコーン側）の先端部を種付けし易いように機械加工したり、所望の直径にするために直胴部に機械加工などが施される。
機械加工が施された原料結晶棒１の表面には不純物が付着しているため、高純度な単結晶を製造するために、一般的にはエッチングや洗浄が行われる。エッチングや洗浄を行い乾燥した後には、表面に再度不純物が付着しないようにするために、原料結晶棒１は包装材で包装される。そしてＦＺ単結晶製造装置３０へ運搬され、チャンバー２０内で上軸３に固定するために上部保持治具４に保持させる作業が行われる。 Normally, the raw material crystal rod 1 needs to be held by the upper holding jig 4 of the upper shaft 3, so that the upper side of the raw material crystal rod 1 (the tail side when it becomes a single crystal) is machined in advance. The tip of the lower side (cone side when it becomes a single crystal) is machined so that it can be easily seeded, or the straight body part is machined to make it a desired diameter.
Since impurities are attached to the surface of the machined raw material crystal rod 1, etching or cleaning is generally performed in order to produce a high-purity single crystal. After etching and cleaning and drying, the raw material crystal rod 1 is packaged with a packaging material in order to prevent impurities from adhering to the surface again. Then, it is transported to the FZ single crystal manufacturing apparatus 30 and is held by the upper holding jig 4 in order to be fixed to the upper shaft 3 in the chamber 20.

このとき、原料結晶棒１を上軸３の上部保持治具４に保持させる作業のために、一旦、図５に示すように、下軸５に設置された円錐形状の凹部１６を有する治具１５に、原料結晶棒１の下部であって、先端部が円錐形状とされた部分を載せて支える。続いて原料結晶棒１の芯出しをしながら上軸３の上部保持治具４に保持させる。 At this time, for the work of holding the raw material crystal rod 1 in the upper holding jig 4 of the upper shaft 3, as shown in FIG. 5, a jig having a conical concave portion 16 installed in the lower shaft 5 once. A portion of the lower portion of the raw material crystal rod 1 having a conical shape at the tip thereof is placed and supported on the fifteenth. Subsequently, the raw material crystal rod 1 is centered and held by the upper holding jig 4 of the upper shaft 3.

ここで、図４に、汎用されている包装材１３を示す。この汎用の包装材１３は筒状の形状をしており、下端部を一直線（平坦）にヒートシール１４を施したものである。このような包装材１３を円錐形状である原料結晶棒１の先端部に被せると、原料結晶棒１の先端部と包装材１３の形状とが大きく異なり一致していないため、図５に示すように、余分な包装材が皺になり、原料結晶棒１の先端部と冶具１５の凹部１６との間に皺の重なり部１８が形成されることとなる。そのため、原料結晶棒１の先端部の円錐形状部の頂部と、冶具１５の凹部１６における円錐頂部１７との位置のずれが大きくなる。その結果、芯出しの調整時に誤差が生じるという問題があった。誤差が許容範囲を超える場合は、修正してやり直さなければならないので、時間が余分に掛かってしまう。 Here, FIG. 4 shows a general-purpose packaging material 13. The general-purpose packaging material 13 has a cylindrical shape, and the lower end portion is straightened (flat) with a heat seal 14. When such a packaging material 13 is put on the tip of the raw material crystal rod 1 having a conical shape, the tip of the raw material crystal rod 1 and the shape of the packaging material 13 are significantly different and do not match, as shown in FIG. In addition, the excess packaging material becomes wrinkled, and the wrinkled overlapping portion 18 is formed between the tip portion of the raw material crystal rod 1 and the recess 16 of the jig 15. Therefore, the displacement between the top of the conical portion at the tip of the raw material crystal rod 1 and the top of the cone 17 in the recess 16 of the jig 15 becomes large. As a result, there is a problem that an error occurs when adjusting the centering. If the error is beyond the permissible range, it will have to be corrected and redone, which will take extra time.

また、芯出しの程度が悪く誤差が大きいと、原料結晶棒１が偏芯して回転するので、絞り工程では絞りが困難になり、場合によっては失敗してしまう。また、絞り工程がうまくできても、その後も常に原料結晶棒１の回転が偏芯しているので、溶融が不均一となり、単結晶が有転位化する確率が増加するという問題があった。
このように、芯出しの誤差をできるだけ小さくする必要があった。 Further, if the degree of centering is poor and the error is large, the raw material crystal rod 1 is eccentric and rotates, which makes it difficult to draw in the drawing step and may fail in some cases. Further, even if the drawing step is successful, the rotation of the raw material crystal rod 1 is always eccentric even after that, so that there is a problem that the melting becomes non-uniform and the probability that the single crystal is dislocated increases.
In this way, it was necessary to reduce the centering error as much as possible.

本発明は、上記問題を解決するためになされたものであり、芯出しの誤差が小さい原料結晶棒の固定方法、及び、不均一な溶融や単結晶の有転位化を抑制できる半導体単結晶の製造方法を提供することを目的とする。また、前記原料結晶棒を包装するための原料結晶棒用包装材を提供することを目的とする。 The present invention has been made to solve the above problems, and is a method for fixing a raw crystal rod having a small centering error, and a semiconductor single crystal capable of suppressing non-uniform melting and dislocation of a single crystal. The purpose is to provide a manufacturing method. Another object of the present invention is to provide a packaging material for a raw material crystal rod for packaging the raw material crystal rod.

本発明は、上記課題を達成するためになされたものであり、原料結晶棒を固定する上軸と種結晶を固定する下軸とを有するＦＺ単結晶製造装置に、先端部が円錐形状とされた原料結晶棒を固定する方法であって、前記原料結晶棒の前記先端部の形状に対応する円錐形状部分を有する包装材を準備する工程と、前記原料結晶棒の前記先端部と前記包装材の前記円錐形状部分とを一致させて、前記原料結晶棒を前記包装材により包装する工程と、前記原料結晶棒の先端部が嵌合する円錐形状の凹部を有する冶具を、前記円錐形状の凹部の円錐頂部と前記下軸の軸中心とが一致するように前記下軸に設置する工程と、前記原料結晶棒が前記包装材により包装された状態で、前記原料結晶棒の前記先端部と前記冶具の前記円錐形状の凹部とを嵌合させることで、前記原料結晶棒を前記下軸に設置された前記冶具に載せて前記原料結晶棒を支える工程と、前記原料結晶棒を前記上軸及び前記下軸に対して芯出ししながら前記上軸に固定する工程とを有することを特徴とする原料結晶棒の固定方法を提供する。 The present invention has been made to achieve the above-mentioned problems, and the FZ single crystal manufacturing apparatus having an upper shaft for fixing a raw crystal rod and a lower shaft for fixing a seed crystal has a conical tip. A method of fixing the raw material crystal rod, which is a step of preparing a packaging material having a conical portion corresponding to the shape of the tip portion of the raw material crystal rod, and a step of preparing the tip portion of the raw material crystal rod and the packaging material. The step of packaging the raw material crystal rod with the packaging material by matching the conical portion of the raw material crystal rod and the jig having a conical concave portion into which the tip end portion of the raw material crystal rod fits are formed into the conical concave portion. The step of installing the raw material crystal rod on the lower shaft so that the top of the cone and the axis center of the lower shaft coincide with each other, and the tip portion of the raw material crystal rod and the tip portion of the raw material crystal rod in a state of being packaged with the packaging material. By fitting the conical recess of the jig, the raw material crystal rod is placed on the jig installed on the lower shaft to support the raw material crystal rod, and the raw material crystal rod is mounted on the upper shaft and the upper shaft. Provided is a method for fixing a raw material crystal rod, which comprises a step of fixing to the upper shaft while centering the lower shaft.

このような原料結晶棒の固定方法によれば、高い精度で原料結晶棒の芯出しを行うことができるようになる。 According to such a method of fixing the raw material crystal rod, it becomes possible to center the raw material crystal rod with high accuracy.

このとき、前記包装材を準備する工程では、包装材の底部にＶ字形にヒートシールを施して、前記原料結晶棒の前記先端部の形状に対応する前記円錐形状部分とすることができる。 At this time, in the step of preparing the packaging material, the bottom of the packaging material can be heat-sealed in a V shape to form the conical portion corresponding to the shape of the tip of the raw material crystal rod.

これにより、より簡便に、原料結晶棒の先端形状に対応する形状の包装材を得ることができる。 Thereby, it is possible to more easily obtain a packaging material having a shape corresponding to the tip shape of the raw material crystal rod.

このとき、前記包装材としてＰＥ（ポリエチレン）製の包装材を用いることができる。 At this time, a PE (polyethylene) packaging material can be used as the packaging material.

これにより、包装材を安価で清浄なものとすることができる。また、ヒートシールがより容易となる。 As a result, the packaging material can be made inexpensive and clean. Also, heat sealing becomes easier.

このとき、前記包装材として少なくとも二重の包装材を用いることが好ましい。 At this time, it is preferable to use at least a double packaging material as the packaging material.

これにより、包装材の穴あき等の破損に基づく原料結晶棒の汚染量をより少なくすることができる。 As a result, the amount of contamination of the raw material crystal rod due to damage such as holes in the packaging material can be further reduced.

このとき、前記芯出しの測定を、レーザー変位計を用いて行うことができる。 At this time, the centering measurement can be performed using a laser displacement meter.

これにより、より精度良く芯出しの程度を測定することができる。 As a result, the degree of centering can be measured more accurately.

そして、原料結晶棒の固定方法により前記原料結晶棒を前記上軸に固定し、さらに前記冶具を取り外すとともに前記包装材を除去し、前記上軸に固定された前記原料結晶棒を誘導加熱コイルで加熱溶融して浮遊帯域を形成し、前記誘導加熱コイルに対して前記原料結晶棒及び前記下軸に固定された種結晶に成長する単結晶棒を回転させながら相対的に下降させ、前記浮遊帯域を移動させることで前記単結晶棒を育成することを特徴とするＦＺ法による半導体単結晶の製造方法が提供される。 Then, the raw material crystal rod is fixed to the upper shaft by the method of fixing the raw material crystal rod, the jig is removed and the packaging material is removed, and the raw material crystal rod fixed to the upper shaft is fixed to the upper shaft by an induction heating coil. The floating zone is formed by heating and melting, and the raw material crystal rod and the single crystal rod that grows into the seed crystal fixed to the lower shaft are relatively lowered while rotating with respect to the induction heating coil. Provided is a method for producing a semiconductor single crystal by an FZ method, which comprises growing the single crystal rod by moving the single crystal rod.

これにより、絞りをより容易に行うことができるとともに、より均一な溶融にできるため、単結晶の有転位化をより抑制することができる。 As a result, the drawing can be performed more easily and the melting can be made more uniform, so that the dislocation of the single crystal can be further suppressed.

また、本発明は、ＦＺ法による半導体単結晶の製造に用いる先端部が円錐形状とされた原料結晶棒を包装するための包装材であって、前記包装材の一部が、前記原料結晶棒の前記先端部の形状に対応する円錐形状部分を有するものであることを特徴とする原料結晶棒用包装材を提供する。 Further, the present invention is a packaging material for packaging a raw material crystal rod having a conical tip portion used for producing a semiconductor single crystal by the FZ method, and a part of the packaging material is the raw material crystal rod. Provided is a packaging material for a raw material crystal rod, which has a conical portion corresponding to the shape of the tip portion of the above.

このような原料結晶棒用包装材によれば、先端が円錐形状とされた結晶原料棒を包装したときの余剰部分を減らすことができ、結晶原料棒の芯出しの精度を高めることが可能なものとなる。 According to such a packaging material for a raw material crystal rod, it is possible to reduce a surplus portion when packaging a crystal raw material rod having a conical tip, and it is possible to improve the accuracy of centering of the crystal raw material rod. It will be a thing.

以上のように、本発明の原料結晶棒の固定方法によれば、高い精度で原料結晶棒の芯出しを行うことができるようになる。また、本発明の原料結晶棒の固定方法を用いて原料結晶棒を上軸に固定しＦＺ法により半導体単結晶を製造することで、絞りをより容易に行うことができるとともに、より均一な溶融にできるため、単結晶の有転位化をより抑制することが可能になる。さらに、本発明の原料結晶棒用包装材によれば、先端が円錐形状とされた結晶原料棒の芯出しの精度を高めることが可能なものとなるとともに、原料先端部で包装材が破断するようなこともない。 As described above, according to the method for fixing the raw material crystal rod of the present invention, the raw material crystal rod can be centered with high accuracy. Further, by fixing the raw material crystal rod to the upper shaft by the method for fixing the raw material crystal rod of the present invention and producing a semiconductor single crystal by the FZ method, drawing can be performed more easily and more uniform melting can be performed. Therefore, it becomes possible to further suppress the dislocation of a single crystal. Further, according to the packaging material for a raw material crystal rod of the present invention, it is possible to improve the accuracy of centering of a crystal raw material rod having a conical tip, and the packaging material breaks at the tip of the raw material. There is no such thing.

ＦＺ単結晶製造装置を示す。The FZ single crystal manufacturing apparatus is shown. 本発明の原料結晶棒用包装材を示す。The packaging material for a raw material crystal rod of this invention is shown. 本発明の原料結晶棒取り付け作業時における、原料結晶棒を冶具に載せた状態図を示す。The state diagram which put the raw material crystal rod on the jig at the time of the raw material crystal rod attachment work of this invention is shown. 汎用（比較例）の包装材を示す。A general-purpose (comparative example) packaging material is shown. 汎用（比較例）の包装材を使用した従来（比較例）の原料結晶棒取り付け作業時における、原料結晶棒を冶具に載せた状態図を示す。The figure which put the raw material crystal rod on a jig at the time of the conventional (comparative example) raw material crystal rod attachment work using the general-purpose (comparative example) packaging material is shown.

以下、本発明を詳細に説明するが、本発明はこれらに限定されるものではない。 Hereinafter, the present invention will be described in detail, but the present invention is not limited thereto.

上述のように、芯出しの誤差が小さい原料結晶棒の固定方法、不均一な溶融や単結晶の有転位化を抑制できる半導体単結晶の製造方法、及び、前記原料結晶棒の固定方法に用いる原料結晶棒用包装材が求められていた。 As described above, it is used in a method for fixing a raw material crystal rod having a small centering error, a method for producing a semiconductor single crystal capable of suppressing non-uniform melting and dislocation of a single crystal, and a method for fixing the raw material crystal rod. There has been a demand for packaging materials for raw crystal rods.

本発明者らは、上記課題について鋭意検討を重ねた結果、原料結晶棒を固定する上軸と種結晶を固定する下軸とを有するＦＺ単結晶製造装置に、先端部が円錐形状とされた原料結晶棒を固定する方法であって、前記原料結晶棒の前記先端部の形状に対応する円錐形状部分を有する包装材を準備する工程と、前記原料結晶棒の前記先端部と前記包装材の前記円錐形状部分とを一致させて、前記原料結晶棒を前記包装材により包装する工程と、前記原料結晶棒の先端部が嵌合する円錐形状の凹部を有する冶具を、前記円錐形状の凹部の円錐頂部と前記下軸の軸中心とが一致するように前記下軸に設置する工程と、前記原料結晶棒が前記包装材により包装された状態で、前記原料結晶棒の前記先端部と前記冶具の前記円錐形状の凹部とを嵌合させることで、前記原料結晶棒を前記下軸に設置された前記冶具に載せて前記原料結晶棒を支える工程と、前記原料結晶棒を前記上軸及び前記下軸に対して芯出ししながら前記上軸に固定する工程とを有する原料結晶棒の固定方法により、高い精度で原料結晶棒の芯出しを行うことができることを見出し、本発明を完成した。 As a result of diligent studies on the above problems, the present inventors have determined that the FZ single crystal manufacturing apparatus having an upper shaft for fixing the raw crystal rod and a lower shaft for fixing the seed crystal has a conical tip. A method of fixing a raw material crystal rod, which is a step of preparing a packaging material having a conical portion corresponding to the shape of the tip portion of the raw material crystal rod, and a step of preparing the tip portion of the raw material crystal rod and the packaging material. The step of packaging the raw material crystal rod with the packaging material by matching the conical portion with the conical portion, and a jig having a conical concave portion into which the tip end portion of the raw material crystal rod fits are provided in the conical concave portion. The step of installing the raw material crystal rod on the lower shaft so that the top of the cone and the axis center of the lower shaft coincide with each other, and the tip portion of the raw material crystal rod and the jig with the raw material crystal rod wrapped in the packaging material. By fitting the conical recess in the above, the raw material crystal rod is placed on the jig installed on the lower shaft to support the raw material crystal rod, and the raw material crystal rod is placed on the upper shaft and the upper shaft. The present invention has been completed by finding that the raw material crystal rod can be centered with high accuracy by the method of fixing the raw material crystal rod having the step of fixing the raw material crystal rod to the upper shaft while centering the lower shaft.

また、ＦＺ法による半導体単結晶の製造に用いる先端部が円錐形状とされた原料結晶棒を包装するための包装材であって、前記包装材の一部が、前記原料結晶棒の前記先端部の形状に対応する円錐形状部分を有する原料結晶棒用包装材により、先端が円錐形状とされた結晶原料棒を包装したときの余剰部分を減らすことができ、結晶原料棒の芯出しの精度を高めることができるものとなることを見出し、本発明を完成した。 Further, it is a packaging material for packaging a raw material crystal rod having a conical tip portion used for manufacturing a semiconductor single crystal by the FZ method, and a part of the packaging material is the tip portion of the raw material crystal rod. With the packaging material for raw crystal raw rods having a conical portion corresponding to the shape of, it is possible to reduce the surplus portion when packaging the crystalline raw material rod having a conical tip, and the accuracy of centering of the crystalline raw material rod can be improved. The present invention has been completed by finding that it can be enhanced.

以下、図面を参照して説明する。 Hereinafter, description will be given with reference to the drawings.

本発明の原料結晶棒の固定方法、半導体単結晶の製造方法で使用するＦＺ単結晶製造装置は、図１に示されるような一般的なＦＺ単結晶製造装置３０が挙げられる。
ＦＺ単結晶製造装置３０は、チャンバー２０内に、原料結晶棒１を固定する上軸３、種結晶８を固定する下軸５、原料結晶棒１を溶融するための誘導加熱コイル７、浮遊帯域１０にガスを吹き付けるガス吹き付け用ノズル１１等を備えている。また、上軸３は原料結晶棒１を保持する上部保持冶具４を含み、下軸５は種結晶８を保持する下部保持冶具６を含んでいる。 Examples of the FZ single crystal manufacturing apparatus used in the method for fixing the raw material crystal rod and the method for manufacturing a semiconductor single crystal of the present invention include a general FZ single crystal manufacturing apparatus 30 as shown in FIG.
The FZ single crystal manufacturing apparatus 30 has an upper shaft 3 for fixing the raw material crystal rod 1, a lower shaft 5 for fixing the seed crystal 8, an induction heating coil 7 for melting the raw material crystal rod 1, and a floating zone in the chamber 20. A gas blowing nozzle 11 or the like for blowing gas to 10 is provided. Further, the upper shaft 3 includes an upper holding jig 4 for holding the raw material crystal rod 1, and the lower shaft 5 includes a lower holding jig 6 for holding the seed crystal 8.

まず、最初に原料結晶棒１であるシリコン原料棒を準備する。シリコン原料棒としては、シーメンス法により製造されたシリコン多結晶棒やＣＺ法により製造されたシリコン単結晶棒などが用いられるが、製造するＦＺ単結晶の仕様に合わせて適宜選択すればよい。 First, a silicon raw material rod, which is a raw material crystal rod 1, is prepared. As the silicon raw material rod, a silicon polycrystalline rod manufactured by the Siemens method, a silicon single crystal rod manufactured by the CZ method, or the like is used, and it may be appropriately selected according to the specifications of the FZ single crystal to be manufactured.

原料結晶棒１は、上側、下側、直胴部などに必要な加工（機械加工等）が施される。特に、結晶製造装置３０に設置されたときに下側となる原料結晶棒１の先端部の形状は、後述の原料結晶棒１の取り付け時の芯出し作業や、種付け時の溶融帯の形成のために、円錐形状に加工される。ここで、本発明において「円錐形状」という場合、先細り状の形状であればよく、正確に円錐形状であるもののみならず、概ね円錐体（略円錐体）と認識されるものが含まれる。 The raw material crystal rod 1 is subjected to necessary processing (machining or the like) on the upper side, the lower side, the straight body portion and the like. In particular, the shape of the tip of the raw material crystal rod 1 that is on the lower side when installed in the crystal manufacturing apparatus 30 is for centering work when the raw material crystal rod 1 is attached, which will be described later, and for forming a melting zone at the time of seeding. Therefore, it is processed into a conical shape. Here, the term "conical shape" in the present invention may be any tapered shape, and includes not only a shape that is exactly a cone but also a shape that is generally recognized as a cone (substantially a cone).

原料結晶棒１に機械加工等を行った後は表面に不純物が付着しているので、高純度な単結晶を製造するために、一般的にはエッチングや洗浄が行われる。エッチングや洗浄を行い乾燥した後には、再度の不純物付着を防止するために、包装材を用いて原料結晶棒１を包装する必要がある。 Since impurities are attached to the surface of the raw material crystal rod 1 after machining or the like, etching or cleaning is generally performed in order to produce a high-purity single crystal. After etching and cleaning and drying, it is necessary to wrap the raw material crystal rod 1 with a packaging material in order to prevent impurities from adhering again.

次に、図２に示すような、包装材１３を準備する工程について説明する。本発明においては、一部が原料結晶棒１の先端部の円錐形状に対応した円錐形状部分１２を有する包装材１３を準備する点に特徴がある。このような円錐形状部分１２を有する包装材１３は、袋やシートなどの汎用の包装材を利用して作製することができる。例えば、図２に示すように、包装材の先端を原料結晶棒１の円錐形状に合わせてＶ字形にヒートシール１４を施すことで、原料結晶棒１の先端部の円錐形状に対応した円錐形状部分１２を有する包装材１３を簡単に作製可能である。ヒートシール１４を施した外側の余分な部分を可能な限りカットすることで、芯出しへの悪影響をさらに小さくすることができる。
なお、包装材１３の円錐形状部分１２の形状は、できるだけ原料結晶棒１の先端部の円錐形状に近いものが好ましいことは当然であるが、必ずしも完全に一致したものに限定されず、形状に多少の違いがあってもよい。 Next, a step of preparing the packaging material 13 as shown in FIG. 2 will be described. The present invention is characterized in that a packaging material 13 having a conical shape portion 12 corresponding to the conical shape of the tip portion of the raw material crystal rod 1 is partially prepared. The packaging material 13 having such a conical portion 12 can be manufactured by using a general-purpose packaging material such as a bag or a sheet. For example, as shown in FIG. 2, the tip of the packaging material is matched with the conical shape of the raw material crystal rod 1 and the heat seal 14 is applied in a V shape to form a conical shape corresponding to the conical shape of the tip of the raw material crystal rod 1. The packaging material 13 having the portion 12 can be easily manufactured. By cutting the excess portion on the outer side to which the heat seal 14 is applied as much as possible, the adverse effect on the centering can be further reduced.
It is natural that the shape of the conical portion 12 of the packaging material 13 is as close as possible to the conical shape of the tip of the raw material crystal rod 1, but the shape is not necessarily limited to a perfect match. There may be some differences.

包装材１３の材質は、ＰＥ（ポリエチレン）が好ましい。ＰＥは厚さ等の種類も多く、適当なシートや袋から選択が容易で安価である。また、添加剤、スリップ剤等を使用していない無添加のＰＥはＣＺ用のチャンクポリなどに一般的に用いられており、不純物汚染が少ないためより好ましい。 The material of the packaging material 13 is preferably PE (polyethylene). There are many types of PE such as thickness, and it is easy to select from suitable sheets and bags and it is inexpensive. Further, additive-free PE that does not use additives, slip agents, or the like is generally used for chunk poly for CZ and the like, and is more preferable because it has less impurity contamination.

また、包装材１３の包装が二重であると、袋が裂けたり、特に原料結晶棒１の先端部と対応する円錐形状部分で穴が開いたりすることを防止できるとともに、原料結晶棒１をチャンバー２０内に搬入する直前に外側の包装材を外すことが出来るので、チャンバー２０に不純物を持ち込む可能性を一段と低くすることができる点で、好ましい。 Further, when the packaging material 13 is double-packed, it is possible to prevent the bag from being torn, and in particular, to prevent a hole from being formed in the conical portion corresponding to the tip portion of the raw material crystal rod 1, and to prevent the raw material crystal rod 1 from being formed. Since the outer packaging material can be removed immediately before being carried into the chamber 20, the possibility of bringing impurities into the chamber 20 can be further reduced, which is preferable.

次に、包装材１３を用いて原料結晶棒１を包装する。このとき、原料結晶棒１の先端部と包装材１３の円錐形状部分１２とを一致させて、包装する。原料結晶棒１の先端部の形状（円錐形状）と、包装材の円錐形状部分１２とは対応する形状であるため、包装材の余剰部分がなくなるか、極めて少なくなる。 Next, the raw material crystal rod 1 is packaged using the packaging material 13. At this time, the tip end portion of the raw material crystal rod 1 and the conical portion 12 of the packaging material 13 are aligned and packaged. Since the shape of the tip portion (conical shape) of the raw material crystal rod 1 and the conical portion 12 of the packaging material have a corresponding shape, the surplus portion of the packaging material is eliminated or extremely reduced.

次に、図３に示すように、原料結晶棒１の取り付け、芯出し等を行うための冶具１５を、下軸５に設置する。この冶具１５には、原料結晶棒１の先端部が嵌合する円錐形状の凹部１６が形成されており、円錐形状の凹部１６における円錐頂部１７が、下軸５の軸中心と一致するように設置する。 Next, as shown in FIG. 3, a jig 15 for attaching the raw material crystal rod 1 and centering the raw material crystal rod 1 is installed on the lower shaft 5. The jig 15 is formed with a conical concave portion 16 into which the tip end portion of the raw material crystal rod 1 is fitted, so that the conical top portion 17 in the conical concave portion 16 coincides with the axis center of the lower shaft 5. Install.

次に、原料結晶棒１をチャンバー２０内に搬入する。図３に示すように、原料結晶棒１が包装材１３により包装された状態で、原料結晶棒１の先端部と下軸５に設置された冶具１５の円錐形状の凹部１６とを嵌合させるようにして、原料結晶棒１を冶具１５に載せて、下軸５により原料結晶棒１を載せて支える。図２に示すような、原料結晶棒１の先端部の円錐形状に対応した円錐形状部分１２を有する包装材１３を使用すると、図５に示すような皺の重なり部１８の発生をなくすか、極めて少なくすることができる。
なお、包装材１３が二重の場合にはチャンバー２０の外で外側の袋を剥がして除去し、内側の包装材１３のみでチャンバー２０の中に運ぶのが好ましい。 Next, the raw material crystal rod 1 is carried into the chamber 20. As shown in FIG. 3, in a state where the raw material crystal rod 1 is packaged by the packaging material 13, the tip end portion of the raw material crystal rod 1 and the conical recess 16 of the jig 15 installed on the lower shaft 5 are fitted. In this way, the raw material crystal rod 1 is placed on the jig 15, and the raw material crystal rod 1 is placed and supported by the lower shaft 5. When the packaging material 13 having the conical shape portion 12 corresponding to the conical shape of the tip portion of the raw material crystal rod 1 as shown in FIG. 2 is used, the occurrence of the wrinkled overlapping portion 18 as shown in FIG. 5 is eliminated. It can be extremely reduced.
When the packaging material 13 is double-layered, it is preferable that the outer bag is peeled off outside the chamber 20 to remove it, and only the inner packaging material 13 is carried into the chamber 20.

続いて、原料結晶棒１を上軸３に固定するために、包装材１３の上部の一部を切断し原料結晶棒１の一部を露出させ、原料結晶棒１の露出した部分を上部保持治具４に保持させる。このときに、保持させるのに必要な最小量だけ包装材１３を剥がすことで、汚染量は最小とできる。そして、上軸３、下軸５に対して芯出しをしながら原料結晶棒１を上部保持治具４に保持させ、上軸３に固定する。 Subsequently, in order to fix the raw material crystal rod 1 to the upper shaft 3, a part of the upper part of the packaging material 13 is cut to expose a part of the raw material crystal rod 1, and the exposed part of the raw material crystal rod 1 is held at the upper part. Hold it in the jig 4. At this time, the amount of contamination can be minimized by peeling off the packaging material 13 by the minimum amount required for holding. Then, while centering the upper shaft 3 and the lower shaft 5, the raw material crystal rod 1 is held by the upper holding jig 4 and fixed to the upper shaft 3.

原料結晶棒１が上軸３に固定されたら上軸３を上方に移動し原料結晶棒１を吊りあげ、包装材１３を剥がし除去する。その後、芯出しの評価を行う。芯出しの評価は結晶を回転させた状態で、先端部の偏芯を目視にて確認することで行っても良いが、レーザー変位計を用いると、芯出しの程度を数値化でき、さらに精度良く芯出しの程度を評価することが出来るので好ましい。原料結晶棒１を回転させて、レーザー変位計により変位を測定すると、偏芯していれば回転に合わせて周期的に変位が変わるので、芯出しの程度を簡便かつ精度よく測定することができる。なお、原料結晶棒１を吊りあげた後に、冶具１５を取り外し、下部保持冶具６を設置する。 When the raw material crystal rod 1 is fixed to the upper shaft 3, the upper shaft 3 is moved upward, the raw material crystal rod 1 is lifted, and the packaging material 13 is peeled off and removed. After that, the centering is evaluated. The centering can be evaluated by visually checking the eccentricity of the tip while the crystal is rotated, but if a laser displacement meter is used, the degree of centering can be quantified and further accuracy is achieved. It is preferable because the degree of centering can be evaluated well. When the raw material crystal rod 1 is rotated and the displacement is measured by a laser displacement meter, if the displacement is eccentric, the displacement changes periodically according to the rotation, so that the degree of centering can be measured easily and accurately. .. After lifting the raw material crystal rod 1, the jig 15 is removed and the lower holding jig 6 is installed.

この後の工程は、通常のＦＺ法による単結晶製造工程と同様である。
図１に示すように、種結晶８を原料結晶棒１の下方に位置する下軸５の下部保持治具６に保持し、誘導加熱コイル７により原料結晶棒１の先端部を溶融して種結晶８に融着させ、その後、種絞りにより絞り部９を形成して無転位化する。そして、浮遊帯域（溶融帯あるいはメルトともいう）１０を原料結晶棒１と単結晶棒２の間に形成し、誘導加熱コイル７に対して、上軸３と下軸５とを回転させながら原料結晶棒１とシリコン単結晶である単結晶棒２を相対的に下降させ、浮遊帯域１０を原料結晶棒１の上端まで移動させてゾーニングし、単結晶棒２を成長させる。なお、この成長は、Ａｒガスに微量の窒素ガスを混合した雰囲気中で行われる。 The subsequent steps are the same as the single crystal manufacturing steps by the usual FZ method.
As shown in FIG. 1, the seed crystal 8 is held by the lower holding jig 6 of the lower shaft 5 located below the raw material crystal rod 1, and the tip portion of the raw material crystal rod 1 is melted by the induction heating coil 7 to melt the seed. It is fused to the crystal 8 and then a dislocation portion 9 is formed by seed drawing to make it dislocation-free. Then, a floating zone (also referred to as a melt zone or melt) 10 is formed between the raw material crystal rod 1 and the single crystal rod 2, and the raw material is rotated with respect to the induction heating coil 7 with the upper shaft 3 and the lower shaft 5. The crystal rod 1 and the single crystal rod 2 which is a silicon single crystal are relatively lowered, and the floating zone 10 is moved to the upper end of the raw material crystal rod 1 for zoning to grow the single crystal rod 2. This growth is performed in an atmosphere in which a small amount of nitrogen gas is mixed with Ar gas.

以下、実施例を挙げて本発明について詳細に説明するが、これは本発明を限定するものではない。 Hereinafter, the present invention will be described in detail with reference to examples, but this is not limited to the present invention.

（実施例）
先端部を先細りの略円錐形状としたシリコン原料棒を、別途準備した図２に示すようなシリコン原料棒の先端部の略円錐形状に対応した略円錐形状部分が形成された包装材を用いて包装し、ＦＺ単結晶製造装置に搬入し、上軸及び下軸に対して芯出しの調整を行いながら、上軸に固定しセットした。
上軸を上昇させてシリコン原料棒を上軸に吊るした後、回転させながらレーザー変位計を用いて偏芯の変位測定を実施した。その後、ＦＺ法によるシリコン結晶棒の製造を行った。この時、絞り形成工程において偏芯が原因で絞り形成が困難となった回数、結晶育成時の偏芯が原因の有転位化の回数をカウントした。
なお、実験は、１００本のシリコン原料棒を用いて行った（Ｎ＝１００）。 (Example)
A silicon raw material rod having a tapered tip portion having a substantially conical shape is prepared using a separately prepared packaging material having a substantially conical shape portion corresponding to the substantially conical shape of the tip portion of the silicon raw material rod as shown in FIG. It was packaged, carried into an FZ single crystal manufacturing apparatus, and fixed to the upper shaft and set while adjusting the centering of the upper shaft and the lower shaft.
After raising the upper shaft and suspending the silicon raw material rod on the upper shaft, the displacement of the eccentricity was measured using a laser displacement meter while rotating. Then, a silicon crystal rod was manufactured by the FZ method. At this time, the number of times that drawing was difficult due to eccentricity in the drawing forming step and the number of dislocations caused by eccentricity during crystal growth were counted.
The experiment was carried out using 100 silicon raw material rods (N = 100).

（比較例）
先端部を先細りの略円錐形状としたシリコン原料棒を、図４に示すような汎用の袋を用いて包装した以外は実施例と同様にして、ＦＺ単結晶製造装置に搬入し、上軸に固定しセットし、その後、ＦＺ法によるシリコン結晶棒の製造を行った。また、実施例と同様の評価を行った。なお、実験は実施例と同様１００本のシリコン原料棒を用いて行った（Ｎ＝１００）。 (Comparative example)
A silicon raw material rod having a substantially conical shape with a tapered tip was carried into the FZ single crystal manufacturing apparatus in the same manner as in the embodiment except that it was packaged using a general-purpose bag as shown in FIG. After fixing and setting, a silicon crystal rod was manufactured by the FZ method. Moreover, the same evaluation as in Example was performed. The experiment was carried out using 100 silicon raw material rods as in the examples (N = 100).

実施例と比較例の評価結果を表１に示す。 Table 1 shows the evaluation results of Examples and Comparative Examples.

Figure 0006996425000001
Figure 0006996425000001

変位測定の結果、シリコン原料棒を回転させたときの変位（偏芯）の平均値は、実施例では０．５ｍｍ、比較例では１．５ｍｍであった。本発明の包装材を使用すると、偏芯の誤差を小さくできることがわかった。 As a result of the displacement measurement, the average value of the displacement (eccentricity) when the silicon raw material rod was rotated was 0.5 mm in the example and 1.5 mm in the comparative example. It was found that the eccentricity error can be reduced by using the packaging material of the present invention.

また、シリコン結晶棒の製造の絞り工程において、シリコン原料棒の偏芯が原因で絞り形成が困難となった回数は実施例では０回、比較例では３回であり、結晶育成時の有転位化の回数も実施例では０回、比較例では１回と、本発明の包装材を使用すると、偏芯が原因で発生する不良の回数をなくすことができた。 Further, in the drawing process of manufacturing the silicon crystal rod, the number of times that drawing was difficult due to the eccentricity of the silicon raw material rod was 0 times in the example and 3 times in the comparative example, and dislocations occurred during crystal growth. The number of crystallizations was 0 in the examples and 1 in the comparative examples. By using the packaging material of the present invention, the number of defects caused by eccentricity could be eliminated.

なお、本発明は、上記実施形態に限定されるものではない。上記実施形態は例示であり、本発明の特許請求の範囲に記載された技術的思想と実質的に同一な構成を有し、同様な作用効果を奏するものは、いかなるものであっても本発明の技術的範囲に包含される。 The present invention is not limited to the above embodiment. The above-described embodiment is an example, and the present invention can be anything that has substantially the same configuration as the technical idea described in the claims of the present invention and exhibits the same function and effect. Is included in the technical scope of.

１…原料結晶棒１、 ２…単結晶棒、 ３…上軸、 ４…上部保持治具、
５…下軸、 ６…下部保持治具、 ７…誘導加熱コイル、 ８…種結晶、
９…絞り部、 １０…浮遊帯域、 １１…ガス吹き付け用ノズル、
１２…円錐形状部分、 １３…包装材、 １４…ヒートシール、
１５…冶具、 １６…円錐形状の凹部、 １７…円錐頂部、 １８…皺の重なり部、
２０…チャンバー、 ３０…ＦＺ単結晶製造装置。 1 ... Raw crystal rod 1, 2 ... Single crystal rod, 3 ... Upper shaft, 4 ... Upper holding jig,
5 ... lower shaft, 6 ... lower holding jig, 7 ... induction heating coil, 8 ... seed crystal,
9 ... Squeezing part, 10 ... Floating zone, 11 ... Gas blowing nozzle,
12 ... Conical part, 13 ... Packaging material, 14 ... Heat seal,
15 ... Jig, 16 ... Conical recess, 17 ... Conical top, 18 ... Overlapping wrinkles,
20 ... Chamber, 30 ... FZ single crystal manufacturing equipment.

Claims (7)

原料結晶棒を固定する上軸と種結晶を固定する下軸とを有するＦＺ単結晶製造装置に、先端部が円錐形状とされた原料結晶棒を固定する方法であって、
前記原料結晶棒の前記先端部の形状に対応する円錐形状部分を有する包装材を準備する工程と、
前記原料結晶棒の前記先端部と前記包装材の前記円錐形状部分とを一致させて、前記原料結晶棒を前記包装材により包装する工程と、
前記原料結晶棒の先端部が嵌合する円錐形状の凹部を有する冶具を、前記円錐形状の凹部の円錐頂部と前記下軸の軸中心とが一致するように前記下軸に設置する工程と、
前記原料結晶棒が前記包装材により包装された状態で、前記原料結晶棒の前記先端部と前記冶具の前記円錐形状の凹部とを嵌合させることで、前記原料結晶棒を前記下軸に設置された前記冶具に載せて前記原料結晶棒を支える工程と、
前記原料結晶棒を前記上軸及び前記下軸に対して芯出ししながら前記上軸に固定する工程とを有することを特徴とする原料結晶棒の固定方法。 A method of fixing a raw crystal rod having a conical tip to an FZ single crystal manufacturing apparatus having an upper shaft for fixing a raw crystal rod and a lower shaft for fixing a seed crystal.
A step of preparing a packaging material having a conical portion corresponding to the shape of the tip portion of the raw material crystal rod, and a step of preparing the packaging material.
A step of matching the tip portion of the raw material crystal rod with the conical portion of the packaging material and packaging the raw material crystal rod with the packaging material.
A step of installing a jig having a conical concave portion into which the tip end portion of the raw material crystal rod is fitted on the lower shaft so that the conical top of the conical concave portion and the axis center of the lower shaft coincide with each other.
With the raw material crystal rod wrapped in the packaging material, the raw material crystal rod is installed on the lower shaft by fitting the tip portion of the raw material crystal rod with the conical concave portion of the jig. The process of supporting the raw material crystal rod by placing it on the jig
A method for fixing a raw material crystal rod, which comprises a step of fixing the raw material crystal rod to the upper shaft while centering the raw material crystal rod with respect to the upper shaft and the lower shaft. 前記包装材を準備する工程では、包装材の底部にＶ字形にヒートシールを施して、前記原料結晶棒の前記先端部の形状に対応する前記円錐形状部分とすることを特徴とする請求項１に記載の原料結晶棒の固定方法。 Claim 1 is characterized in that, in the step of preparing the packaging material, the bottom portion of the packaging material is heat-sealed in a V shape to form the conical portion corresponding to the shape of the tip portion of the raw material crystal rod. The method for fixing a raw material crystal rod according to. 前記包装材としてＰＥ（ポリエチレン）製の包装材を用いることを特徴とする請求項１または請求項２に記載の原料結晶棒の固定方法。 The method for fixing a raw material crystal rod according to claim 1 or 2, wherein a PE (polyethylene) packaging material is used as the packaging material. 前記包装材として少なくとも二重の包装材を用いることを特徴とする請求項１から請求項３のいずれか一項に記載の原料結晶棒の固定方法。 The method for fixing a raw material crystal rod according to any one of claims 1 to 3, wherein at least a double packaging material is used as the packaging material. 前記芯出しの評価を、レーザー変位計を用いて行うことを特徴とする請求項１から請求項４のいずれか一項に記載の原料結晶棒の固定方法。 The method for fixing a raw material crystal rod according to any one of claims 1 to 4, wherein the centering is evaluated using a laser displacement meter. 請求項１から請求項５のいずれか一項に記載の原料結晶棒の固定方法により前記原料結晶棒を前記上軸に固定し、さらに前記冶具を取り外すとともに前記包装材を除去し、
前記上軸に固定された前記原料結晶棒を誘導加熱コイルで加熱溶融して浮遊帯域を形成し、前記誘導加熱コイルに対して前記原料結晶棒及び前記下軸に固定された種結晶に成長する単結晶棒を回転させながら相対的に下降させ、前記浮遊帯域を移動させることで前記単結晶棒を育成することを特徴とするＦＺ法による半導体単結晶の製造方法。 The raw material crystal rod is fixed to the upper shaft by the method for fixing the raw material crystal rod according to any one of claims 1 to 5, and further, the jig is removed and the packaging material is removed.
The raw material crystal rod fixed to the upper shaft is heated and melted by an induction heating coil to form a floating zone, and grows into the raw material crystal rod and a seed crystal fixed to the lower shaft with respect to the induction heating coil. A method for producing a semiconductor single crystal by the FZ method, which comprises growing a single crystal rod by relatively lowering the single crystal rod while rotating it and moving the floating zone. ＦＺ法による半導体単結晶の製造に用いる先端部が円錐形状とされた原料結晶棒を包装するための包装材であって、
前記包装材の一部が、前記原料結晶棒の前記先端部の形状に対応する円錐形状部分を有するものであることを特徴とする原料結晶棒用包装材。 A packaging material for packaging a raw crystal rod having a conical tip, which is used for manufacturing a semiconductor single crystal by the FZ method.
A packaging material for a raw material crystal rod, wherein a part of the packaging material has a conical portion corresponding to the shape of the tip portion of the raw material crystal rod.
JP2018105046A 2018-05-31 2018-05-31 Method for fixing raw material crystal rods, method for manufacturing semiconductor single crystals, and packaging materials for raw material crystal rods Active JP6996425B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2018105046A JP6996425B2 (en) 2018-05-31 2018-05-31 Method for fixing raw material crystal rods, method for manufacturing semiconductor single crystals, and packaging materials for raw material crystal rods

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2018105046A JP6996425B2 (en) 2018-05-31 2018-05-31 Method for fixing raw material crystal rods, method for manufacturing semiconductor single crystals, and packaging materials for raw material crystal rods

Publications (2)

Publication Number Publication Date
JP2019210163A JP2019210163A (en) 2019-12-12
JP6996425B2 true JP6996425B2 (en) 2022-01-17

Family

ID=68846289

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2018105046A Active JP6996425B2 (en) 2018-05-31 2018-05-31 Method for fixing raw material crystal rods, method for manufacturing semiconductor single crystals, and packaging materials for raw material crystal rods

Country Status (1)

Country Link
JP (1) JP6996425B2 (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014031283A (en) 2012-08-01 2014-02-20 Shin Etsu Handotai Co Ltd Method for producing semiconductor single crystal rod by floating zone method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014031283A (en) 2012-08-01 2014-02-20 Shin Etsu Handotai Co Ltd Method for producing semiconductor single crystal rod by floating zone method

Also Published As

Publication number Publication date
JP2019210163A (en) 2019-12-12

Similar Documents

Publication Publication Date Title
KR20180101586A (en) Manufacturing method of silicon single crystal
JP2005306653A (en) Method for manufacturing silicon single crystal
US20090293804A1 (en) Method of shoulder formation in growing silicon single crystals
JP2003313089A (en) Method for manufacturing single crystal silicon and single crystal silicon wafer, seed crystal for manufacturing single crystal silicon, single crystal silicon ingot, and single crystal silicon wafer
JP2006248825A (en) Silicon carbide ingot and its manufacturing method
EP2679706B1 (en) Method for manufacturing n-type silicon single crystal
US20090260564A1 (en) Method for growing silicon single crystal
JP6248816B2 (en) Single crystal manufacturing method
JP6996425B2 (en) Method for fixing raw material crystal rods, method for manufacturing semiconductor single crystals, and packaging materials for raw material crystal rods
EP1722014A1 (en) Method for manufacturing nitrogen-doped silicon single crystal
JP5318365B2 (en) Silicon crystal material and method for producing FZ silicon single crystal using the same
US20090293803A1 (en) Method of growing silicon single crystals
KR20150071850A (en) Gas discharge pipe and ingot growing apparatus having the same
US20090293802A1 (en) Method of growing silicon single crystals
KR101751789B1 (en) Silicon single crystal ingot and method for growing the same
JP6007892B2 (en) Method for producing silicon single crystal
JP2011184213A (en) Method for producing silicon single crystal
JP5924181B2 (en) Manufacturing method of FZ single crystal silicon
KR20190100653A (en) Method for correcting shape of silicon single crystal ingot
EP4190949A1 (en) Crucible for cz
JPH07157391A (en) Production of silicon single crystal excellent in oxidized film pressure resistance and device thereof
TWI836994B (en) Ingot piece of silicon containing dopant
JP4341379B2 (en) Single crystal manufacturing method
JP6954083B2 (en) Method for manufacturing silicon raw material rod for FZ and method for manufacturing FZ silicon single crystal
JP6777013B2 (en) Single crystal manufacturing method

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20210217

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20211029

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20211116

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20211129

R150 Certificate of patent or registration of utility model

Ref document number: 6996425

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150