JPH09235186A - Seed crystal for lifting single crystal and lifting of single crystal with the seed crystal - Google Patents
Seed crystal for lifting single crystal and lifting of single crystal with the seed crystalInfo
- Publication number
- JPH09235186A JPH09235186A JP4376496A JP4376496A JPH09235186A JP H09235186 A JPH09235186 A JP H09235186A JP 4376496 A JP4376496 A JP 4376496A JP 4376496 A JP4376496 A JP 4376496A JP H09235186 A JPH09235186 A JP H09235186A
- Authority
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- Prior art keywords
- seed crystal
- single crystal
- pulling
- crystal
- seed
- 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.)
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Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、単結晶引き上げ用
種結晶及び該種結晶を用いた単結晶の引き上げ方法に関
し、より詳細にはチョクラルスキー法（以下、ＣＺ法と
記す）等により、シリコン等からなる単結晶を引き上げ
る際に用いられる、単結晶引き上げ用種結晶及び該種結
晶を用いた単結晶の引き上げ方法に関する。TECHNICAL FIELD The present invention relates to a seed crystal for pulling a single crystal and a method for pulling a single crystal using the seed crystal, more specifically, by the Czochralski method (hereinafter referred to as CZ method) or the like. The present invention relates to a seed crystal for pulling a single crystal used when pulling a single crystal made of silicon or the like and a method for pulling a single crystal using the seed crystal.
【０００２】[0002]
【従来の技術】現在、ＬＳＩ（大規模集積回路）等の回
路素子形成用基板として使用されているシリコン単結晶
の大部分は、ＣＺ法により引き上げられたシリコン単結
晶が用いられている。図２は、このＣＺ法に用いられる
単結晶引き上げ装置を模式的に示した断面図であり、図
中１１は坩堝を示している。2. Description of the Related Art At present, most of silicon single crystals used as substrates for forming circuit elements such as LSIs (Large Scale Integrated Circuits) are silicon single crystals pulled by the CZ method. FIG. 2 is a cross-sectional view schematically showing a single crystal pulling apparatus used in this CZ method, and 11 in the figure shows a crucible.
【０００３】この坩堝１１は、有底円筒形状の石英製坩
堝１１ａと、この石英製坩堝１１ａの外側に嵌合され
た、同じく有底円筒形状の黒鉛製坩堝１１ｂとから構成
されており、坩堝１１は、図中の矢印方向に所定の速度
で回転する支持軸１８に支持されている。この坩堝１１
の外側には、抵抗加熱式のヒータ１２、ヒータ１２の外
側には保温筒１７が同心円状に配置されており、坩堝１
１内には、このヒータ１２により溶融させた結晶用原料
の溶融液１３が、充填されるようになっている。また、
坩堝１１の中心軸上には、引き上げ棒あるいはワイヤー
等からなる引き上げ軸１４が吊設されており、この引き
上げ軸１４の先にシードチャック１４ａを介して単結晶
引き上げ用種結晶３５（以下、単に種結晶とも記す）が
取り付けられるようになっている。また、これら部材
は、圧力の制御が可能な水冷式のチャンバ１９内に納め
られている。The crucible 11 comprises a bottomed cylindrical quartz crucible 11a and a bottomed cylindrical graphite crucible 11b fitted to the outside of the quartz crucible 11a. 11 is supported by a support shaft 18 that rotates at a predetermined speed in the direction of the arrow in the figure. This crucible 11
A resistance heating type heater 12 is provided outside the heater 12, and a heat insulating cylinder 17 is concentrically arranged outside the heater 12.
The melt 1 of the raw material for crystallization melted by the heater 12 is filled in the inside 1. Also,
A pulling shaft 14 made of a pulling rod, a wire, or the like is hung on the central axis of the crucible 11, and a seed crystal 35 for pulling a single crystal (hereinafter, simply referred to as a pulling shaft 14 via a seed chuck 14a is provided. (Also referred to as a seed crystal) is attached. Further, these members are housed in a water-cooled chamber 19 whose pressure can be controlled.
【０００４】上記した単結晶引き上げ装置により単結晶
３６を引き上げる方法を、図２及び図３に基づいて説明
する。図３（ａ）〜（ｄ）は、単結晶を引き上げる各工
程のうちの、一部の工程における種結晶の近傍を、模式
的に示した部分拡大正面図である。A method of pulling the single crystal 36 by the above-mentioned single crystal pulling apparatus will be described with reference to FIGS. 2 and 3. 3A to 3D are partially enlarged front views schematically showing the vicinity of the seed crystal in some of the steps of pulling the single crystal.
【０００５】図３には示していないが、まずヒータ１２
により結晶用原料を溶融させ、チャンバ１９内を減圧し
た後、しばらく放置して溶融液１３中のガスを十分に放
出させ、その後、不活性ガスを導入してチャンバ１９内
を減圧の不活性ガス雰囲気とする。Although not shown in FIG. 3, first, the heater 12
The raw material for crystallization is melted by means of to reduce the pressure in the chamber 19 and then left for a while to sufficiently release the gas in the melt 13, and then an inert gas is introduced to reduce the pressure in the chamber 19 to the inert gas. The atmosphere.
【０００６】次に、支持軸１８と同一軸心で逆方向に所
定の速度で引き上げ軸１４を回転させながら、引き上げ
軸１４の先に取り付けられた種結晶３５を降下させて溶
融液１３に着液させ、種結晶３５を溶融液１３に馴染ま
せた後、単結晶３６の引き上げを開始する（以下、この
工程をシーディング工程と記す）（図３（ａ））。Next, while rotating the pulling shaft 14 in the opposite direction with the same axis as the supporting shaft 18 at a predetermined speed, the seed crystal 35 attached to the tip of the pulling shaft 14 is lowered to reach the melt 13. After the liquid crystal is made to melt and the seed crystal 35 is made to adapt to the melt liquid 13, pulling up of the single crystal 36 is started (hereinafter, this step is referred to as a seeding step) (FIG. 3A).
【０００７】次に、種結晶３５の先端に結晶を成長させ
るが、このとき後述するメインボディ３６ｃ形成速度よ
り早い速度で引き上げ軸１４を引き上げ、所定径になる
まで結晶を細く絞り、ネック３６ａを形成する（以下、
この工程をネッキング工程と記す）（図３（ｂ）。Next, a crystal is grown on the tip of the seed crystal 35. At this time, the pulling shaft 14 is pulled up at a speed faster than the main body 36c forming speed, which will be described later, and the crystal is narrowed down to a predetermined diameter, and the neck 36a is opened. Form (hereinafter,
This step is referred to as a necking step) (FIG. 3B).
【０００８】次に、単結晶３６の引き上げ速度（以下、
単に引き上げ速度とも記す）を落して単結晶３６を所定
の径まで成長させ、ショルダー３６ｂを形成する（以
下、この工程をショルダー形成工程と記す）（図３
（ｃ））。Next, the pulling speed of the single crystal 36 (hereinafter,
The single crystal 36 is grown to a predetermined diameter by lowering the pulling rate (also simply referred to as a pulling rate) to form a shoulder 36b (hereinafter, this step is referred to as a shoulder forming step) (FIG. 3).
(C)).
【０００９】次に、一定の速度で単結晶３６を引き上げ
ることにより、一定の径、所定長さのメインボディ３６
ｃを形成する（以下、この工程をメインボディ３６ｃ形
成工程と記す）（図３（ｄ））。Next, by pulling the single crystal 36 at a constant speed, the main body 36 having a constant diameter and a predetermined length.
c is formed (hereinafter, this step is referred to as a main body 36c forming step) (FIG. 3D).
【００１０】さらに、図３には示していないが、最後に
急激な温度変化により単結晶３６に高密度の転位が導入
されないよう、単結晶３６の直径を徐々に絞って単結晶
３６全体の温度を徐々に降下させ、終端コーンを形成し
た後、単結晶３６を溶融液１３から切り離す。前記工程
の後冷却して、単結晶３６の引き上げが完了する。Although not shown in FIG. 3, finally, the diameter of the single crystal 36 is gradually reduced so that a high-density dislocation is not introduced into the single crystal 36 due to a sudden temperature change. Is gradually lowered to form a terminal cone, and then the single crystal 36 is separated from the melt 13. After the above steps, the single crystal 36 is pulled down and cooled down.
【００１１】上記単結晶３６の引き上げにおける重要な
工程として、上記ネッキング工程（図３（ｂ））があ
る。そこで、上記ネッキング工程を行う目的について以
下に説明する。まず上記シーディング工程（図３
（ａ））を行うにあたって、種結晶底部３５ａは、ある
程度予熱された後に溶融液１３に着液されるが、この予
熱の温度（約１３００℃程度以下）と種結晶３５の融点
（約１４１０℃）との間には、１００℃以上の差があ
る。従って、溶融液１３への着液時に種結晶３５は急激
に温度が上昇し、種結晶底部３５ａには、熱応力による
転位が発生する。該転位は、単結晶化を阻害するもので
あるため、前記転位を排除してから単結晶３６を成長さ
せる必要がある。一般に前記転位は、単結晶３６の成長
界面に対して垂直方向に成長する傾向があることから、
上記ネッキング工程により前記成長界面（ネック３６ａ
の先端面）の形状を、図３（ｂ）に示したように下に凸
形状とし、前記転位を排除する。The necking step (FIG. 3B) is an important step in pulling the single crystal 36. Therefore, the purpose of performing the necking step will be described below. First, the seeding step (see FIG. 3)
In carrying out (a)), the seed crystal bottom portion 35a is preheated to some extent and then comes into contact with the melt 13, but the temperature of this preheating (about 1300 ° C. or lower) and the melting point of the seed crystal 35 (about 1410 ° C.). ), There is a difference of 100 ° C. or more. Therefore, the temperature of the seed crystal 35 rapidly rises when the liquid crystal 13 reaches the melt 13, and dislocations due to thermal stress occur in the seed crystal bottom portion 35a. Since the dislocations inhibit single crystallization, it is necessary to grow the single crystal 36 after eliminating the dislocations. Generally, the dislocations tend to grow in a direction perpendicular to the growth interface of the single crystal 36,
The growth interface (neck 36a) is formed by the necking process.
As shown in FIG. 3 (b), the shape of the front end surface of the is made convex downward to eliminate the dislocation.
【００１２】また、上記ネッキング工程においては、引
き上げ速度を高速にするほど、ネック３６ａの径を細く
することができ、前記成長界面の形状をより下に凸とし
て、前記転位の伝播を抑制することができ、前記転位を
効率良く排除することができる。Further, in the necking step, the diameter of the neck 36a can be made smaller as the pulling speed is increased, and the growth interface is made to have a downwardly convex shape to suppress the propagation of the dislocation. The dislocation can be efficiently eliminated.
【００１３】[0013]
【発明が解決しようとする課題】上記した従来の単結晶
の引き上げ方法においては、直径が約６インチ、重量が
８０ｋｇ程度の単結晶３６を引き上げるために、直径約
１２ｍｍの種結晶３５を用いるのが一般的であった。そ
の際、単結晶３６を安全に支持するためには、ネック３
６ａの径が大きい方がよく、他方転位を効率的に排除す
るためにはネック３６ａの径はできるだけ小さい方がよ
い。これら両者の要求を満たすネック３６ａの直径とし
て、３ｍｍ程度が選択されていた。しかしながら、近年
の半導体デバイスの高集積化、低コスト化及び生産性の
効率化に対応して、ウエハも大口径化が要求されてきて
おり、最近では、例えば直径約１２インチ（３００ｍ
ｍ）、重量が３００ｋｇ程度の単結晶３６の製造が望ま
れている。この場合、従来のネック３６ａの直径（通常
３ｍｍ程度）では、ネック３６ａが引き上げられる単結
晶３６の重さに耐えられずに破損し、単結晶３６が落下
してしまうという課題があった。In the conventional method of pulling a single crystal, the seed crystal 35 having a diameter of about 12 mm is used to pull the single crystal 36 having a diameter of about 6 inches and a weight of about 80 kg. Was common. At this time, in order to support the single crystal 36 safely, the neck 3
The diameter of 6a is preferably large, while the diameter of neck 36a is preferably as small as possible in order to eliminate dislocations efficiently. A diameter of about 3 mm was selected as the diameter of the neck 36a satisfying these requirements. However, in response to the recent trend of higher integration of semiconductor devices, cost reduction, and efficiency improvement of productivity, the wafer is also required to have a large diameter, and recently, for example, a diameter of about 12 inches (300 m) is required.
m), it is desired to manufacture a single crystal 36 having a weight of about 300 kg. In this case, with the diameter of the conventional neck 36a (usually about 3 mm), the neck 36a is not able to withstand the weight of the pulled single crystal 36 and is damaged, causing the single crystal 36 to drop.
【００１４】上記した大重量の単結晶３６を製造するに
あたり、単結晶３６の落下等の事故の発生を防ぎ、安全
に引き上げを行うためには、シリコン強度（約１６ｋｇ
ｆ／ｍｍ2 ）から算出して、ネック３６ａの直径を約６
ｍｍとする必要がある。しかしながら、ネック３６ａの
直径を約６ｍｍ以上にすると、種結晶３５の溶融液１３
への着液時に生じた転位を、十分に排除することができ
ない。In manufacturing the above-mentioned heavy-weight single crystal 36, in order to prevent accidents such as dropping of the single crystal 36 and to pull up safely, the silicon strength (about 16 kg
f / mm 2 ) and the diameter of the neck 36a is about 6
It must be mm. However, when the diameter of the neck 36a is about 6 mm or more, the melt 13 of the seed crystal 35 is
It is not possible to sufficiently eliminate the dislocations that have occurred during the contact with the liquid.
【００１５】本発明は、上記課題に鑑みなされたもので
あり、単結晶を成長させる際の着液時に、種結晶自体に
転位が導入されず、従って、ネッキング工程を省略する
ことができる、単結晶引き上げ用種結晶を提供すること
を目的としている。また、本発明は、前記単結晶引き上
げ用種結晶を用い、ネックを形成せしなくとも転位を伝
播させず、大重量の単結晶であっても安全にかつ低コス
トで単結晶を引き上げることができる単結晶の引き上げ
方法を提供することをも、目的としている。The present invention has been made in view of the above problems, and dislocations are not introduced into the seed crystal itself at the time of landing when growing a single crystal, and therefore, the necking step can be omitted. It is intended to provide a seed crystal for pulling a crystal. Further, the present invention uses the seed crystal for pulling a single crystal, does not propagate dislocations without forming a neck, and is capable of pulling a single crystal safely and at low cost even with a heavy single crystal. It is also an object to provide a method for pulling a single crystal that can be performed.
【００１６】[0016]
【課題を解決するための手段及びその効果】上記目的を
達成するために、本発明に係る単結晶引き上げ用種結晶
（１）は、円柱形状の胴体部と円錐形状の先端部とを有
することを特徴としている。In order to achieve the above object, the seed crystal for pulling a single crystal according to the present invention (1) has a cylindrical body and a conical tip. Is characterized by.
【００１７】上記構成の単結晶引き上げ用種結晶（１）
によれば、該種結晶の先端部が円錐形状であり、その熱
容量が小さくなっているので、前記種結晶を余熱して溶
融液に着液させる際に、先端付近が容易に溶融液の温度
近くになり、温度の急変（熱ショック）で発生する転位
の導入を防止することができる。そのため、ネックを形
成しなくとも、転位を伝播させることなく単結晶を引き
上げることができ、従来よりも重い重量の単結晶を引き
上げる場合においても、十分に単結晶を支持することが
できる。また、前記種結晶は、単結晶を上記形状に加工
することにより、容易に作製することができ、かつネッ
ク形成の必要がないため、種結晶全体の大きさを通常の
引き上げ方法の場合と比較して小さくすることができ、
種結晶の製造コストを削減することができる。Seed crystal (1) for pulling a single crystal having the above structure
According to the method, since the tip portion of the seed crystal has a conical shape and its heat capacity is small, when the seed crystal is preheated and allowed to land on the melt, the temperature near the tip easily melts near the tip. It becomes close, and it is possible to prevent the introduction of dislocation which occurs due to a sudden temperature change (heat shock). Therefore, the single crystal can be pulled without propagating dislocations without forming a neck, and the single crystal can be sufficiently supported even when pulling a heavier weight single crystal than in the past. Further, the seed crystal can be easily produced by processing a single crystal into the above shape, and since it is not necessary to form a neck, the size of the whole seed crystal is compared with that in the case of a normal pulling method. Can be made smaller,
The manufacturing cost of the seed crystal can be reduced.
【００１８】また、本発明に係る単結晶引き上げ用種結
晶（２）は、上記（１）記載の単結晶引き上げ用種結晶
において、円柱形状の胴体部の直径が６ｍｍ以上あるこ
とを特徴としている。Further, the seed crystal for pulling a single crystal according to the present invention (2) is characterized in that, in the seed crystal for pulling a single crystal according to the above (1), the diameter of the cylindrical body portion is 6 mm or more. .
【００１９】上記構成の単結晶引き上げ用種結晶（２）
によれば、円柱形状の胴体部の直径が６ｍｍ以上と十分
に大きいので、メインボディの直径が約１２インチで、
重量が３００ｋｇ程度の大重量の単結晶を引き上げる場
合においても、前記単結晶の胴体部分は、前記単結晶を
十分に支持することができる。Seed crystal (2) for pulling a single crystal having the above structure
According to the above, the diameter of the cylindrical body is 6 mm or more, which is sufficiently large, so that the main body has a diameter of about 12 inches.
Even when pulling a large-weight single crystal having a weight of about 300 kg, the body portion of the single crystal can sufficiently support the single crystal.
【００２０】また、本発明に係る単結晶の引き上げ方法
（１）は、上記単結晶引き上げ用種結晶（１）又は
（２）を用い、該単結晶引き上げ用種結晶の先端部を溶
融液に浸漬して溶かし込んだ後、ネックを形成せずに単
結晶を引き上げることを特徴としている。In the method (1) for pulling a single crystal according to the present invention, the seed crystal (1) or (2) for pulling a single crystal is used, and the tip of the seed crystal for pulling a single crystal is made into a melt. The feature is that the single crystal is pulled up without forming a neck after being immersed and melted.
【００２１】上記単結晶の引き上げ方法（１）によれ
ば、安価な上記単結晶引き上げ用種結晶（１）又は
（２）を用い、着液時に該種結晶に転位を導入させるこ
となく、引き上げに十分な強度を有する径の部分まで溶
解させることができる。従って、ネックを形成せずに単
結晶を引き上げることができ、大重量の単結晶であって
も安全にかつ低コストで引き上げることができる。According to the above single crystal pulling method (1), the inexpensive single crystal pulling up seed crystal (1) or (2) is used, and the pulling up is performed without introducing dislocation into the seed crystal at the time of landing. It is possible to dissolve even a portion having a diameter having sufficient strength. Therefore, the single crystal can be pulled without forming a neck, and even a single crystal having a large weight can be pulled safely and at low cost.
【００２２】また、本発明に係る単結晶の引き上げ方法
（２）は、上記単結晶の引き上げ方法（１）において、
溶かし込み後の単結晶引き上げ用種結晶の先端部分の直
径が、６ｍｍ以上あることを特徴としている。The method (2) for pulling a single crystal according to the present invention is the same as the method (1) for pulling a single crystal described above.
The diameter of the tip portion of the seed crystal for pulling the single crystal after melting is 6 mm or more.
【００２３】上記単結晶の引き上げ方法（２）によれ
ば、メインボディの直径が約１２インチで、重量が３０
０ｋｇ程度の大重量の単結晶であっても、安全にかつ低
コストで引き上げることができる。According to the above single crystal pulling method (2), the main body has a diameter of about 12 inches and a weight of 30.
Even a single crystal having a large weight of about 0 kg can be pulled safely and at low cost.
【００２４】[0024]
【発明の実施の形態】以下、本発明に係る単結晶引き上
げ用種結晶及び該種結晶を用いた単結晶の引き上げ方法
の実施の形態を、図面に基づいて説明する。BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of a seed crystal for pulling a single crystal and a method for pulling a single crystal using the seed crystal according to the present invention will be described below with reference to the drawings.
【００２５】実施の形態に係る単結晶の引き上げ方法に
用いる装置は、特に限定されるものではなく、ＣＺ法に
用いられる単結晶引き上げ装置（図２）であってもよ
く、溶融層法に用いられる単結晶引き上げ装置であって
もよい。また、実施の形態に係る単結晶の引き上げ方法
は１２インチ以上の大口径、大重量の単結晶の引き上げ
を前提としている。The apparatus used in the method for pulling a single crystal according to the embodiment is not particularly limited, and may be a single crystal pulling apparatus (FIG. 2) used in the CZ method, which is used in the melt layer method. It may be a single crystal pulling apparatus used. Further, the single crystal pulling method according to the embodiment is premised on pulling a single crystal having a large diameter of 12 inches or more and a large weight.
【００２６】本実施の形態では、図２に示した単結晶引
き上げ装置を用いて単結晶の引き上げを行った場合につ
いて説明するので、ここでは、単結晶引き上げ装置自体
の説明は省略する。In the present embodiment, the case of pulling a single crystal by using the single crystal pulling apparatus shown in FIG. 2 will be described, so that the description of the single crystal pulling apparatus itself will be omitted here.
【００２７】図１（ａ）〜（ｄ）は、実施の形態に係る
単結晶の引き上げ方法の一部の工程における種結晶の近
傍を、模式的に示した部分拡大正面図である。FIGS. 1A to 1D are partially enlarged front views schematically showing the vicinity of a seed crystal in a part of the steps of the single crystal pulling method according to the embodiment.
【００２８】図１（ａ）に、種結晶１５の一部を示して
いるが、種結晶１５は円柱形状の胴体部１５ａと、円錐
形状の先端部１５ｂとを含んで構成されている。この胴
体部１５ａの直径は６〜３０ｍｍが好ましく、先端部１
５ｂの長さ（ｈ）は５〜１００ｍｍが好ましい。胴体部
１５ａの直径が６ｍｍ未満であると、後述する工程にお
ける、種結晶１５の溶かし込み時の先端部１５ｂの直径
を、６ｍｍ以上に設定するのが困難となり、１２インチ
以上の直径で３００ｋｇを超える重量の単結晶１６を支
持するのが難しくなり、他方、胴体部１５ａの直径が３
０ｍｍを超えると、種結晶１５が大きすぎて経済的に不
利となる。また、先端部１５ｂの長さ（ｈ）が５ｍｍ未
満では、後述する工程における着液時に、種結晶１５に
熱応力による転位が導入され易くなり、他方先端部１５
ｂの長さ（ｈ）が１００ｍｍを超えると、先端部１５ｂ
の溶かし込みに時間がかかりすぎる。FIG. 1A shows a part of the seed crystal 15. The seed crystal 15 is composed of a cylindrical body portion 15a and a conical tip portion 15b. The body portion 15a preferably has a diameter of 6 to 30 mm, and the tip portion 1
The length (h) of 5b is preferably 5 to 100 mm. If the diameter of the body portion 15a is less than 6 mm, it will be difficult to set the diameter of the tip portion 15b when the seed crystal 15 is melted in the step described later to 6 mm or more, and 300 kg for a diameter of 12 inches or more. It becomes difficult to support the single crystal 16 having an excess weight, while the diameter of the body portion 15a is 3
If it exceeds 0 mm, the seed crystal 15 is too large, which is economically disadvantageous. If the length (h) of the tip portion 15b is less than 5 mm, dislocations due to thermal stress are likely to be introduced into the seed crystal 15 at the time of landing in the process described later, while the other tip portion 15b is formed.
When the length (h) of b exceeds 100 mm, the tip portion 15b
It takes too long to melt.
【００２９】次に、実施の形態に係る単結晶の引き上げ
方法を説明するが、下記の工程以前の工程は、「従来の
技術」の項で説明した方法と同様の方法で行う。Next, a method of pulling a single crystal according to the embodiment will be described. The steps prior to the following steps are performed by the same method as the method described in the section "Prior Art".
【００３０】支持軸１８と同一軸心で逆方向に所定の速
度で引き上げ軸１４を回転させながら、シードチャック
１４ａに取り付けられた、胴体部１５ａが円柱形状で先
端部１５ｂが円錐形状の種結晶１５を、溶融液１３直上
まで降下させて種結晶１５の予熱を行う（図２、図１
（ａ））。While rotating the pulling shaft 14 in the opposite direction at the same axis as the supporting shaft 18 at a predetermined speed, the seed crystal having a cylindrical body 15a and a conical tip 15b attached to the seed chuck 14a. 15 is lowered to directly above the melt 13 to preheat the seed crystal 15 (see FIGS. 2 and 1).
(A)).
【００３１】予熱時間を５〜１２０分程度とることによ
り、種結晶１５の先端部１５ｂの温度が上昇し、先端部
１５ｂの溶融液１３に近い部分は、ほぼ溶融液１３の温
度となる。このときの溶融液１３と種結晶１５の最先端
との距離は、１〜３０ｍｍ程度が好ましい。By setting the preheating time to about 5 to 120 minutes, the temperature of the tip portion 15b of the seed crystal 15 rises, and the portion of the tip portion 15b near the melt 13 becomes almost the temperature of the melt 13. At this time, the distance between the melt 13 and the tip of the seed crystal 15 is preferably about 1 to 30 mm.
【００３２】次に、種結晶１５を降下させ、種結晶１５
の先端部１５ｂを溶融液１３の表面に着液させる（図１
（ｂ））。この着液時に、種結晶１５の先端部１５ｂは
ほぼ溶融液１３の温度となっているので、種結晶１５に
温度差に起因する熱応力は発生せず、転位が導入される
こともない。Next, the seed crystal 15 is lowered to form the seed crystal 15
The front end portion 15b of the molten liquid 13 is applied to the surface of the melt 13 (see FIG. 1).
(B)). At the time of this liquid deposition, the tip portion 15b of the seed crystal 15 is almost at the temperature of the melt 13, so that thermal stress due to the temperature difference does not occur in the seed crystal 15 and dislocations are not introduced.
【００３３】次に、種結晶１５を０．５〜２ｍｍ／分の
速度で降下させ、種結晶１５の先端部１５ｂの一部を溶
かし込む（図１（ｃ））。種結晶１５の降下速度が０．
５ｍｍ／分未満であると、先端部１５ｂを溶融させるの
に時間がかかりすぎ、他方種結晶１５の降下速度が２ｍ
ｍ／分を超えると、先端部１５ｂを完全に溶融液１３に
溶かし込むことが困難となる。また、先端部１５ｂを溶
かし込んだ時に残留する、先端部１５ｂの底部１５０ｂ
の直径は、６ｍｍ以上あることが好ましい。底部１５０
ｂの直径が６ｍｍ未満の場合には、メインボディ１６ｂ
の直径が１２インチ程度で、重量が３００ｋｇ程度の大
重量の単結晶１６を支持するのが難しくなる。Next, the seed crystal 15 is lowered at a speed of 0.5 to 2 mm / min to melt a part of the tip portion 15b of the seed crystal 15 (FIG. 1 (c)). The descending speed of the seed crystal 15 is 0.
If it is less than 5 mm / min, it takes too much time to melt the tip portion 15b, while the descending speed of the seed crystal 15 is 2 m.
When it exceeds m / min, it becomes difficult to completely dissolve the tip portion 15b into the melt 13. Further, the bottom portion 150b of the tip portion 15b, which remains when the tip portion 15b is melted, is left.
The diameter is preferably 6 mm or more. Bottom 150
If the diameter of b is less than 6 mm, the main body 16b
It is difficult to support the heavy single crystal 16 having a diameter of about 12 inches and a weight of about 300 kg.
【００３４】この後、溶融液１３の温度を調整し、ネッ
クを形成することなく、ショルダー１６ａ形成工程及び
メインボディ１６ｂ形成工程を行う。すなわち、所定の
引き上げ速度で単結晶１６を所定の径（約１２インチ）
まで成長させてショルダー１６ａを形成し、所定の引き
上げ速度で単結晶１６を引き上げて、メインボディ１６
ｂを形成する（図１（ｄ））。After that, the temperature of the melt 13 is adjusted, and the shoulder 16a forming step and the main body 16b forming step are performed without forming a neck. That is, the single crystal 16 is set to a predetermined diameter (about 12 inches) at a predetermined pulling rate.
To form a shoulder 16a, and pulling the single crystal 16 at a predetermined pulling speed,
b is formed (FIG. 1D).
【００３５】その後は、「従来の技術」の項で説明した
方法と同様の方法により単結晶１６を引き上げ、溶融液
１３から切り離して冷却させることにより、単結晶１６
の引き上げを完了する。After that, the single crystal 16 is pulled by a method similar to the method described in the section "Prior Art", separated from the melt 13 and cooled, whereby the single crystal 16 is removed.
Complete the pull up.
【００３６】[0036]
【実施例及び比較例】以下、実施例に係る単結晶引き上
げ用種結晶、及び該種結晶を用いた単結晶の引き上げ方
法を説明する。また、比較例として、従来の単結晶引き
上げ用種結晶を用い、従来の方法で単結晶の引き上げを
行った場合についても説明する。以下、その条件を記載
する。EXAMPLES AND COMPARATIVE EXAMPLES Hereinafter, a seed crystal for pulling a single crystal according to an example and a method for pulling a single crystal using the seed crystal will be described. Further, as a comparative example, a case where a conventional single crystal pulling seed crystal is used and the single crystal is pulled by the conventional method will be described. The conditions will be described below.
【００３７】＜実施例１及び比較例１〜２に共通の条件
＞ 引き上げる単結晶１６の形状 直径：約３００ｍｍ（１２インチ）、長さ：約１０００
ｍｍ、重量：約２７０ｋｇ 結晶用原料の仕込み量：３００ｋｇ チャンバ１９内の雰囲気：Ａｒ雰囲気 Ａｒの流量：８０リットル／分 圧力：１．３３×１０3 Ｐａ 引き上げ軸１４の回転速度：２０ｒｐｍ 坩堝１１の回転速度：５ｒｐｍ 引き上げ回数：各実施例及び比較例につき１０回 ＜実施例１の場合の条件＞ 種結晶１５の形状：円柱形状の胴体部１５ａと円錐形状
の先端部１５ｂとを有する（図１）。 胴体部１５ａの直径：１２ｍｍ、胴体部１５ａの長さ：
７０ｍｍ 先端部１５ｂの長さ（ｈ）：６０ｍｍ 予熱時の種結晶１５の最先端の位置：溶融液１３の直
上１ｍｍ 着液後の種結晶１５の降下速度：０．７ｍｍ／分 溶かし込みにより残留した先端部１５ｂの底部１５０
ｂの直径：１０ｍｍ ショルダー１６ａ形成時の単結晶１６の引き上げ速
度：０．３ｍｍ／分 メインボディ１６ｂ形成時の単結晶１６の引き上げ速
度：０．５ｍｍ／分 ＜比較例１の場合の条件＞ 種結晶３５の形状：円柱形状 直径：１２ｍｍ、長さ：７０ｍｍ 予熱時の種結晶底部３５ａの位置：溶融液１３の直上
１ｍｍ 着液後、ネック３６ａ形成時の引き上げ速度：３．０
ｍｍ／分 ネック３６ａの最小径部分の直径：４ｍｍ ショルダー３６ｂ形成時の引き上げ速度：０．３ｍｍ
／分 メインボディ３６ｃ形成時の引き上げ速度：０．５ｍ
ｍ／分 ＜比較例２の場合の条件＞ 種結晶３５の形状：円柱形状 直径：１２ｍｍ、長さ：７０ｍｍ 予熱時の種結晶底部３５ａの位置：溶融液１３の直上
１ｍｍ 着液後、ネック３６ａ形成時の引き上げ速度：４．０
ｍｍ／分 ネック３６ａの最小径部分の直径：１０ｍｍ ショルダー３６ｂ形成時の引き上げ速度：０．３ｍｍ
／分 メインボディ３６ｃ形成時の引き上げ速度：０．５ｍ
ｍ／分 ＜引き上げた単結晶のＤＦ（Dislocation Free) 率の調
査方法＞引き上げた単結晶１６、３６を成長方向（長さ
方向）に平行にスライスし、得られた単結晶１６、３６
のＸ線トポグラフを測定し、その結果より判断した。す
なわち、Ｘ線トポグラフより少しでも転位が認められた
単結晶１６、３６は、転位ありと判断し、引き上げた単
結晶１０本のうち、転位のない（ＤＦ）ものの割合を調
べた。<Conditions Common to Example 1 and Comparative Examples 1 and 2> Shape of Single Crystal 16 to be Pulled Diameter: about 300 mm (12 inches), Length: about 1000
mm, weight: about 270 kg Amount of raw material for crystallization: 300 kg Atmosphere in chamber 19: Ar atmosphere Ar flow rate: 80 liter / min Pressure: 1.33 × 10 3 Pa Rotation speed of pulling shaft 14: 20 rpm of crucible 11 Rotation speed: 5 rpm Number of times of pulling up: 10 times for each example and comparative example <Conditions for Example 1> Shape of seed crystal 15: cylindrical body 15a and conical tip 15b (Fig. 1) ). Diameter of body 15a: 12 mm, length of body 15a:
70 mm Length of the tip portion 15b (h): 60 mm Position of the tip of the seed crystal 15 at the time of preheating: 1 mm directly above the melt 13 Descent rate of the seed crystal 15 after landing: 0.7 mm / min Remained by melting Bottom portion 150 of the end portion 15b
Diameter of b: 10 mm Pulling speed of the single crystal 16 when forming the shoulder 16a: 0.3 mm / min Pulling speed of the single crystal 16 when forming the main body 16b: 0.5 mm / min <Conditions for Comparative Example 1> Seed Shape of crystal 35: cylindrical shape Diameter: 12 mm, length: 70 mm Position of seed crystal bottom portion 35a during preheating: 1 mm directly above the melt 13 After pulling liquid, pulling up speed during neck 36a formation: 3.0
mm / min Diameter of the smallest diameter portion of the neck 36a: 4 mm Pulling speed when forming the shoulder 36b: 0.3 mm
/ Min Pulling speed when forming the main body 36c: 0.5 m
m / min <Conditions for Comparative Example 2> Shape of seed crystal 35: cylindrical shape Diameter: 12 mm, length: 70 mm Position of seed crystal bottom 35a during preheating: 1 mm directly above the melt 13 Neck 36a after landing Lifting speed during formation: 4.0
mm / min Diameter of the smallest diameter portion of the neck 36a: 10 mm Pulling speed when forming the shoulder 36b: 0.3 mm
/ Min Pulling speed when forming the main body 36c: 0.5 m
m / min <Investigation method of DF (Dislocation Free) rate of pulled single crystal> The pulled single crystals 16 and 36 were sliced parallel to the growth direction (length direction), and the obtained single crystals 16 and 36 were obtained.
X-ray topograph was measured and judged from the results. That is, it was judged that the single crystals 16 and 36 in which dislocations were recognized even a little from the X-ray topography had dislocations, and the ratio of dislocation-free (DF) out of the 10 pulled single crystals was examined.
【００３８】＜実施例１、及び比較例１〜２の結果＞上
記実施例１及び比較例１〜２の場合の、単結晶１６、３
６のＤＦ率及び落下数を下記の表１に示す。<Results of Example 1 and Comparative Examples 1 and 2> Single crystals 16 and 3 in the case of Example 1 and Comparative Examples 1 and 2 above.
The DF ratio and the number of drops of No. 6 are shown in Table 1 below.
【００３９】[0039]
【表１】 [Table 1]
【００４０】上記表１に示す結果より明らかなように、
実施例１の場合には、種結晶１５に転位が導入されない
ため、ネック３６ａ（図３）を形成せずに引き上げて
も、引き上げた単結晶１６のＤＦ率は９０％（９／１
０）と殆ど転位が発生していない。また種結晶１５の先
端部１５ｂを溶かし込んだ時の、先端部１５ｂの直径が
１０ｍｍと十分に太いので、落下数は０／１０であっ
た。As is clear from the results shown in Table 1 above,
In the case of Example 1, since dislocations were not introduced into the seed crystal 15, even if the single crystal 16 was pulled up without forming the neck 36a (FIG. 3), the DF ratio of the pulled single crystal 16 was 90% (9/1).
0), almost no dislocations occurred. Further, when the tip portion 15b of the seed crystal 15 was melted, the diameter of the tip portion 15b was sufficiently thick as 10 mm, and the number of drops was 0/10.
【００４１】これに対し、比較例１の場合には、ネック
３６ａの直径が４ｍｍになるまでその径を絞ったので、
ＤＦ率は９０％（９／１０）と良好であったが、単結晶
３６を十分に支持することができず、落下数が８／１０
と、殆どのものが落下していまった。また、比較例２の
場合には、ネック３６ａの直径を１０ｍｍと太くしたた
め、落下数は０／１０であったが、種結晶３５に導入さ
れた転位を排除することができず、ＤＦ率が０％（０／
１０）と、全ての単結晶３６に転位が発生してしまっ
た。On the other hand, in the case of Comparative Example 1, since the diameter of the neck 36a was reduced to 4 mm,
The DF ratio was 90% (9/10), which was good, but the single crystal 36 could not be sufficiently supported and the number of drops was 8/10.
And almost everything fell off. Further, in the case of Comparative Example 2, the diameter of the neck 36a was thickened to 10 mm, so the number of drops was 0/10, but the dislocations introduced into the seed crystal 35 could not be eliminated, and the DF ratio was 0% (0 /
10), dislocations occurred in all the single crystals 36.
【図１】（ａ）〜（ｄ）は、本発明の実施の形態に係る
単結晶の引き上げ方法の工程の一部を、模式的に示した
部分拡大正面図である。FIG. 1A to FIG. 1D are partially enlarged front views schematically showing some of the steps of a method for pulling a single crystal according to an embodiment of the present invention.
【図２】ＣＺ法において使用される単結晶引き上げ装置
を、模式的に示した断面図である。FIG. 2 is a sectional view schematically showing a single crystal pulling apparatus used in the CZ method.
【図３】（ａ）〜（ｄ）は、従来の単結晶の引き上げ方
法の工程の一部を、模式的に示した部分拡大正面図であ
る。3 (a) to 3 (d) are partially enlarged front views schematically showing a part of the steps of the conventional method for pulling a single crystal.
１５ 種結晶 １５ａ 胴体部 １５ｂ 先端部 １６ 単結晶 15 seed crystal 15a body part 15b tip part 16 single crystal
Claims (4)
を有することを特徴とする単結晶引き上げ用種結晶。1. A seed crystal for pulling a single crystal, which has a cylindrical body and a conical tip.
ることを特徴とする請求項１記載の単結晶引き上げ用種
結晶。2. The seed crystal for pulling a single crystal according to claim 1, wherein the cylindrical body has a diameter of 6 mm or more.
上げ用種結晶を用い、該単結晶引き上げ用種結晶の先端
部を溶融液に浸漬して溶かし込んだ後、ネックを形成せ
ずに単結晶を引き上げることを特徴とする単結晶の引き
上げ方法。3. A single crystal pulling seed crystal according to claim 1 is used, and a neck is not formed after the tip of the single crystal pulling seed crystal is immersed in a melt and melted. A method for pulling a single crystal, which comprises pulling the single crystal into
の先端部分の直径が６ｍｍ以上あることを特徴とする請
求項３記載の単結晶の引き上げ方法。4. The method for pulling a single crystal according to claim 3, wherein the diameter of the tip portion of the seed crystal for pulling the single crystal after melting is 6 mm or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8043764A JP3016126B2 (en) | 1996-02-29 | 1996-02-29 | Single crystal pulling method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8043764A JP3016126B2 (en) | 1996-02-29 | 1996-02-29 | Single crystal pulling method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09235186A true JPH09235186A (en) | 1997-09-09 |
| JP3016126B2 JP3016126B2 (en) | 2000-03-06 |
Family
ID=12672833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8043764A Expired - Fee Related JP3016126B2 (en) | 1996-02-29 | 1996-02-29 | Single crystal pulling method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3016126B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0930381A1 (en) * | 1998-01-14 | 1999-07-21 | Shin-Etsu Handotai Company Limited | Method of producing a silicon monocrystal |
| EP0949361A2 (en) * | 1998-04-07 | 1999-10-13 | Shin-Etsu Handotai Company Limited | Silicon seed crystal for the Czochralski method and method for producing a silicon single crystal |
| US6197108B1 (en) | 1997-05-21 | 2001-03-06 | Shin-Etsu Handotai, Co. Ltd. | Silicon seed crystal, method of manufacturing the same, and method of manufacturing silicon monocrystal through use of the seed crystal |
| US6866713B2 (en) | 2001-10-26 | 2005-03-15 | Memc Electronic Materials, Inc. | Seed crystals for pulling single crystal silicon |
| JP2009298641A (en) * | 2008-06-12 | 2009-12-24 | Sumco Corp | Silicon single crystal and method for manufacturing the same |
| JP2010095425A (en) * | 2008-10-20 | 2010-04-30 | Shin Etsu Handotai Co Ltd | Method for producing silicon single crystal |
| WO2013088646A1 (en) * | 2011-12-16 | 2013-06-20 | 信越半導体株式会社 | Method for producing silicon single crystal |
| CN115110146A (en) * | 2022-06-30 | 2022-09-27 | 西安奕斯伟材料科技有限公司 | Seed crystal and crystal pulling method and device |
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1996
- 1996-02-29 JP JP8043764A patent/JP3016126B2/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6197108B1 (en) | 1997-05-21 | 2001-03-06 | Shin-Etsu Handotai, Co. Ltd. | Silicon seed crystal, method of manufacturing the same, and method of manufacturing silicon monocrystal through use of the seed crystal |
| EP0930381A1 (en) * | 1998-01-14 | 1999-07-21 | Shin-Etsu Handotai Company Limited | Method of producing a silicon monocrystal |
| EP0949361A2 (en) * | 1998-04-07 | 1999-10-13 | Shin-Etsu Handotai Company Limited | Silicon seed crystal for the Czochralski method and method for producing a silicon single crystal |
| EP0949361A3 (en) * | 1998-04-07 | 2000-02-02 | Shin-Etsu Handotai Company Limited | Silicon seed crystal for the Czochralski method and method for producing a silicon single crystal |
| US6670036B2 (en) | 1998-04-07 | 2003-12-30 | Shin-Etsu Handotai Co., Ltd. | Silicon seed crystal and method for producing silicon single crystal |
| US6866713B2 (en) | 2001-10-26 | 2005-03-15 | Memc Electronic Materials, Inc. | Seed crystals for pulling single crystal silicon |
| JP2009298641A (en) * | 2008-06-12 | 2009-12-24 | Sumco Corp | Silicon single crystal and method for manufacturing the same |
| JP2010095425A (en) * | 2008-10-20 | 2010-04-30 | Shin Etsu Handotai Co Ltd | Method for producing silicon single crystal |
| WO2013088646A1 (en) * | 2011-12-16 | 2013-06-20 | 信越半導体株式会社 | Method for producing silicon single crystal |
| JP2013126926A (en) * | 2011-12-16 | 2013-06-27 | Shin Etsu Handotai Co Ltd | Method for producing silicon single crystal |
| US9476142B2 (en) | 2011-12-16 | 2016-10-25 | Shin-Etsu Handotai Co., Ltd. | Method for manufacturing silicon single crystal |
| CN115110146A (en) * | 2022-06-30 | 2022-09-27 | 西安奕斯伟材料科技有限公司 | Seed crystal and crystal pulling method and device |
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