JP2013133230A - Method for producing silicon single crystal - Google Patents
Method for producing silicon single crystal Download PDFInfo
- Publication number
- JP2013133230A JP2013133230A JP2011282412A JP2011282412A JP2013133230A JP 2013133230 A JP2013133230 A JP 2013133230A JP 2011282412 A JP2011282412 A JP 2011282412A JP 2011282412 A JP2011282412 A JP 2011282412A JP 2013133230 A JP2013133230 A JP 2013133230A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- measuring unit
- distance measuring
- silica glass
- glass crucible
- 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.)
- Granted
Links
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 49
- 239000010703 silicon Substances 0.000 title claims abstract description 49
- 239000013078 crystal Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000005259 measurement Methods 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 238000009826 distribution Methods 0.000 claims abstract description 5
- 230000003746 surface roughness Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 20
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 239000000843 powder Substances 0.000 description 11
- 239000000377 silicon dioxide Substances 0.000 description 11
- 230000007704 transition Effects 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010314 arc-melting process Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003703 image analysis method Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
本発明は、シリコン単結晶の製造方法に関する。 The present invention relates to a method for producing a silicon single crystal.
シリコン単結晶の製造にはシリカガラスルツボを用いたチョクラルスキー法（ＣＺ法）が採用されている。具体的には、シリカガラスルツボの内部にシリコン多結晶原料を熔融したシリコン融液を貯留し、シリコン単結晶の種結晶を接触させ、回転させながら徐々に引き上げ、シリコン単結晶の種結晶を核として成長させてシリコン単結晶を製造する。 A Czochralski method (CZ method) using a silica glass crucible is employed for producing a silicon single crystal. Specifically, a silicon melt obtained by melting a silicon polycrystal raw material is stored inside a silica glass crucible, and a silicon single crystal seed crystal is brought into contact with the silicon crystal crucible and is gradually pulled up to rotate the silicon single crystal seed crystal as a nucleus. To produce a silicon single crystal.
シリコン単結晶引き上げに用いるルツボには、円筒状の側壁部と、湾曲した底部と、前記側壁部と前記底部を連結し且つ前記底部よりも曲率が大きいコーナー部を備えるものがある。このようなルツボを用いて引き上げを行う場合、シリコン融液の液面が側壁部に位置している間は、液面の低下速度はゆっくりで且つ一定となるので有転移化が起こりにくい。しかし、シリコン融液の液面が側壁部とコーナー部の境界に到達し、そこからさらに低下すると液面の低下速度が大きくなり且つその速度が不規則になる。そのようになるのは、コーナー部は大きな曲率を有しているので液面が低下すると伴ってその面積が急速に縮小することと、コーナー部は、その形状のバラツキが比較的大きくなりやすい部位であり、そのため１つ１つのルツボでコーナー部の形状が厳密には異なっていることが要因である。 Some crucibles used for pulling a silicon single crystal include a cylindrical side wall portion, a curved bottom portion, and a corner portion that connects the side wall portion and the bottom portion and has a larger curvature than the bottom portion. When pulling up using such a crucible, while the liquid level of the silicon melt is located at the side wall, the rate of decrease of the liquid level is slow and constant, so that transition is unlikely to occur. However, if the surface of the silicon melt reaches the boundary between the side wall portion and the corner portion and further decreases from there, the rate of decrease in the liquid level increases and the rate becomes irregular. This is because the corner portion has a large curvature, so that the area rapidly decreases as the liquid level decreases, and the corner portion is subject to a relatively large variation in shape. For this reason, the shape of the corner portion is strictly different between each crucible.
特許文献１においては、コーナー部での有転移化を防ぐために、シリコン融液の液面がコーナー部に到達する前にシリコン単結晶の直胴部の成長を終了させている。 In Patent Document 1, in order to prevent transition at the corner portion, the growth of the straight body portion of the silicon single crystal is terminated before the liquid surface of the silicon melt reaches the corner portion.
しかし、特許文献１の方法は、シリコン単結晶の直胴部の長さを犠牲にしているという問題があるので、シリコン単結晶の直胴部の長さを犠牲することなく有転移化を防ぐ技術が望まれている。 However, since the method of Patent Document 1 has a problem that the length of the straight body portion of the silicon single crystal is sacrificed, the transition is prevented without sacrificing the length of the straight body portion of the silicon single crystal. Technology is desired.
本発明はこのような事情に鑑みてなされたものであり、シリカガラスルツボのコーナー部においてもシリコン単結晶の引き上げを適切に行うことを可能にするシリコン単結晶の製造方法を提供するものである。 The present invention has been made in view of such circumstances, and provides a method for producing a silicon single crystal that makes it possible to appropriately pull up the silicon single crystal even in a corner portion of a silica glass crucible. .
本発明によれば、円筒状の側壁部と、湾曲した底部と、前記側壁部と前記底部を連結し且つ前記底部よりも曲率が大きいコーナー部を備えるシリカガラスルツボ内に保持されたシリコン融液からシリコン単結晶を引き上げる工程を備え、前記シリコン融液の液面が前記コーナー部に到達した後の前記シリコン単結晶の引き上げ条件が、前記シリカガラスルツボの内表面の三次元形状に基づいて決定され、前記内表面の表面粗さの三次元分布は、前記シリカガラスルツボの内表面に沿って非接触で内部測距部を移動させ、移動経路上の複数の測定点において、内部測距部から前記シリカガラスルツボの内表面に対して斜め方向にレーザー光を照射し、前記内表面からの内表面反射光を検出することによって、内部測距部と前記内表面の間の内表面距離を測定し、各測定点の三次元座標と、前記内表面距離を関連付けることによって、前記シリカガラスルツボの内表面の三次元形状を求める工程を備える方法によって決定される、シリコン単結晶の製造方法が提供される。 According to the present invention, a silicon melt held in a silica glass crucible having a cylindrical side wall portion, a curved bottom portion, and a corner portion connecting the side wall portion and the bottom portion and having a larger curvature than the bottom portion. A step of pulling up the silicon single crystal from the substrate, and the pulling condition of the silicon single crystal after the surface of the silicon melt reaches the corner is determined based on the three-dimensional shape of the inner surface of the silica glass crucible. The three-dimensional distribution of the surface roughness of the inner surface moves the inner distance measuring unit in a non-contact manner along the inner surface of the silica glass crucible, and the inner distance measuring unit at a plurality of measurement points on the moving path. By irradiating laser light in an oblique direction to the inner surface of the silica glass crucible, and detecting the inner surface reflected light from the inner surface, the inner surface between the internal distance measuring unit and the inner surface Manufacturing a silicon single crystal determined by a method comprising measuring a distance and determining a three-dimensional shape of the inner surface of the silica glass crucible by associating the three-dimensional coordinates of each measurement point with the inner surface distance A method is provided.
上記の通り、シリコン融液の液面がコーナー部に到達した後に引き上げでは有転移化が非常に起こりやすいため、従来技術のように液面がコーナー部に到達する前に引き上げを終了させてしまうか、又は熟練した作業者が勘に従って引き上げ速度を調節して有転移化を防いでいるのが現状である。前者の場合、シリコン融液の無駄が発生してシリコン単結晶の製造コスト上昇に繋がり、後者の場合、引き上げ工程の自動化の妨げになり、人件費の上昇に繋がり、やはり製造コストの上昇に繋がる。 As described above, the transition is very likely to occur when the silicon melt reaches the corner after the liquid level reaches the corner, so the lifting ends before the liquid reaches the corner as in the prior art. Or, the current situation is that a skilled worker prevents the transition by adjusting the pulling speed according to intuition. In the former case, waste of the silicon melt is generated, leading to an increase in the manufacturing cost of the silicon single crystal, and in the latter case, the automation of the pulling process is hindered, leading to an increase in labor costs, which also leads to an increase in manufacturing cost. .
そこで、本発明者らは、従来とは発想を転換し、予めルツボの内表面の３次元形状を測定しておくことによって、コーナー部での液面の下降速度を高精度に予測し、その予測内容に基づいてシリコン単結晶の引き上げ速度などの引き上げ条件を決定することを可能にし、それによって有転移化を防ぎ且つ引き上げの自動化を可能にするという発明を完成させた。
本発明は、外径２８インチ以上の大型ルツボや、４０インチ以上の超大型ルツボにおいて特に利点がある。なぜなら、このようなルツボにおいては、引き上げに失敗した場合の損失が非常に大きいので、引き上げ条件の最適設定の重要性が特に高いからである。
Therefore, the present inventors changed the idea from the prior art, and by predicting the three-dimensional shape of the inner surface of the crucible in advance, predicting the descending speed of the liquid level at the corner with high accuracy, The present invention has been completed, which makes it possible to determine pulling conditions such as the pulling speed of a silicon single crystal based on the predicted contents, thereby preventing transition and allowing the pulling to be automated.
The present invention is particularly advantageous in a large crucible having an outer diameter of 28 inches or more and a super large crucible having a diameter of 40 inches or more. This is because, in such a crucible, since the loss when the pulling fails is very large, the importance of the optimum setting of the pulling conditions is particularly high.
全てのルツボの内表面形状が設計図通りになるのであれば、ルツボの内表面の三次元形状は設計図面を見るだけで特定することができるが、実際には、シリカガラスルツボの内表面形状は、ルツボ毎に異なるので、１つ１つのルツボについてルツボの内表面の三次元形状を特定することが必須である。 If the inner surface shape of all the crucibles is as shown in the design drawing, the three-dimensional shape of the inner surface of the crucible can be specified only by looking at the design drawing, but in reality, the inner surface shape of the silica glass crucible. Therefore, it is essential to specify the three-dimensional shape of the inner surface of the crucible for each crucible.
本発明者らは、通常の三次元レーザースキャナを用いて、内表面の三次元形状を特定しようとしたが、ルツボが透明体であるので、測定はうまくいかなかった。ルツボ内表面に光を照射して画像を取得し、その画像を解析する方法も試してみたが、この方法では、画像の解析に非常に長い時間がかかるため、ルツボの内表面全体の三次元形状の測定には到底使えるものではなかった。 The present inventors tried to specify the three-dimensional shape of the inner surface using a normal three-dimensional laser scanner, but the measurement was not successful because the crucible was a transparent body. I tried to illuminate the inner surface of the crucible to acquire an image and analyze the image, but this method takes a very long time to analyze the image. It could not be used to measure the shape.
このような状況において、本発明者らは、ルツボの内表面に対して斜め方向からレーザー光を照射したところ、ルツボ内表面からの反射光（内表面反射光）の検出が可能であり、この反射光に基づいて内部測距部と内表面の間の内表面距離が測定可能であることを見出した。 In such a situation, the present inventors can detect the reflected light (inner surface reflected light) from the inner surface of the crucible when the inner surface of the crucible is irradiated with laser light from an oblique direction. It was found that the inner surface distance between the inner distance measuring unit and the inner surface can be measured based on the reflected light.
また、ルツボの内表面に沿った複数の測定点において測定が行われるが、各測定点での内部測距部の座標と内表面距離を関連付けることによって、各測定点に対応するルツボ内表面座標が得られる。 In addition, the measurement is performed at a plurality of measurement points along the inner surface of the crucible. By associating the inner surface distance with the coordinates of the internal distance measuring unit at each measurement point, the inner surface coordinates of the crucible corresponding to each measurement point. Is obtained.
そして、ルツボの内表面に沿って、例えば２ｍｍ間隔のメッシュ状に多数の測定点を配置して測定を行うことによって、メッシュ状の内表面座標が得られ、これによって、ルツボの内表面の三次元形状を求めることができる。
この方法が優れているのは、画像解析による方法に比べて、データのサンプリングレートが格段に大きいことであり、予備実験によると、直径１ｍのルツボで１０万点の測定をする場合であっても、１０分程度で内表面全体の三次元形状の測定を終えることができた。
Then, along the inner surface of the crucible, for example, by arranging a large number of measurement points in a mesh shape with an interval of 2 mm and performing measurement, the mesh-like inner surface coordinates are obtained, thereby obtaining the tertiary of the inner surface of the crucible. The original shape can be obtained.
The superiority of this method is that the data sampling rate is much higher than that of the image analysis method. According to a preliminary experiment, 100,000 points are measured with a 1 m diameter crucible. However, the measurement of the three-dimensional shape of the entire inner surface was completed in about 10 minutes.
以下、本発明の種々の実施形態を例示する。以下の実施形態は、互いに組み合わせ可能である。 Hereinafter, various embodiments of the present invention will be exemplified. The following embodiments can be combined with each other.
好ましくは、内部測距部からのレーザー光は、前記内表面に対して３０〜６０度の入射角で照射される。 Preferably, the laser beam from the internal distance measuring unit is irradiated at an incident angle of 30 to 60 degrees with respect to the inner surface.
好ましくは、内部測距部は、内部測距部を三次元的に移動させることができるように構成された内部ロボットアームに固定され、前記シリカガラスルツボは、内部ロボットアームを覆うように配置される。 Preferably, the internal distance measuring unit is fixed to an internal robot arm configured to be able to move the internal distance measuring unit three-dimensionally, and the silica glass crucible is disposed so as to cover the internal robot arm. The
以下、図１〜図５を用いて、本発明の一実施形態のシリコン単結晶の製造方法を説明する。 Hereinafter, a method for manufacturing a silicon single crystal according to an embodiment of the present invention will be described with reference to FIGS.
＜１．シリカガラスルツボ＞
本発明の一実施形態のシリコン単結晶の製造方法で使用されるシリカガラスルツボ１１は、一例では、回転モールドの内表面に平均粒径３００μｍ程度のシリカ粉を堆積させてシリカ粉層を形成するシリカ粉層形成工程と、モールド側からシリカ粉層を減圧しながら、シリカ粉層をアーク熔融させることによってシリカガラス層を形成するアーク熔融工程を備える（この方法を「回転モールド法」と称する）方法によって製造される。
<1. Silica glass crucible>
In one example, the silica glass crucible 11 used in the method for producing a silicon single crystal according to an embodiment of the present invention forms a silica powder layer by depositing silica powder having an average particle size of about 300 μm on the inner surface of a rotary mold. A silica powder layer forming step and an arc melting step of forming a silica glass layer by arc melting the silica powder layer while reducing the pressure of the silica powder layer from the mold side (this method is referred to as “rotary molding method”) Manufactured by the method.
アーク熔融工程の初期にはシリカ粉層を強く減圧することによって気泡を除去して透明シリカガラス層（以下、「透明層」と称する。）１３を形成し、その後、減圧を弱くすることによって気泡が残留した気泡含有シリカガラス層（以下、「気泡含有層」と称する。）１５を形成することによって、内表面側に透明層１３を有し、外表面側に気泡含有層１５を有する二層構造のシリカガラスルツボを形成することができる。 At the initial stage of the arc melting process, the silica powder layer is strongly decompressed to remove bubbles to form a transparent silica glass layer (hereinafter referred to as “transparent layer”) 13, and then the decompression is weakened to reduce the bubbles. Forming a bubble-containing silica glass layer 15 (hereinafter referred to as “bubble-containing layer”) 15, thereby having two layers having a transparent layer 13 on the inner surface side and a bubble-containing layer 15 on the outer surface side. A structured silica glass crucible can be formed.
ルツボの製造に使用されるシリカ粉には、天然石英を粉砕して製造される天然シリカ粉や化学合成によって製造される合成シリカ粉があるが、特に天然シリカ粉は、天然物を原料としているので、物性・形状・サイズがばらつきやすい。物性・形状・サイズが変化すると、シリカ粉の熔融状態が変化するので、同じ条件でアーク熔融を行っても、製造されるルツボの内表面形状がばらついてしまう。従って、内表面形状は、一つ一つのルツボについて測定する必要がある。 Silica powder used for crucible production includes natural silica powder produced by pulverizing natural quartz and synthetic silica powder produced by chemical synthesis, but natural silica powder is made from natural products. Therefore, physical properties, shapes, and sizes tend to vary. When the physical properties, shape, and size change, the melting state of the silica powder changes, so that the inner surface shape of the manufactured crucible varies even when arc melting is performed under the same conditions. Therefore, the inner surface shape needs to be measured for each crucible.
シリカガラスルツボ１１は、円筒状の側壁部１１ａと、湾曲した底部１１ｃと、側壁部１１ａと底部１１ｃを連結し且つ底部１１ｃよりも曲率が大きいコーナー部１１ｂを備える。本発明において、コーナー部１１ｂとは、側壁部１１ａと底部１１ｃを連接する部分で、コーナー部の曲線の接線がシリカガラスルツボの側壁部１１ａと重なる点から、底部１１ｃと共通接線を有する点までの部分のことを意味する。言い換えると、シリカガラスルツボ１１の側壁部１１ａが曲がり始める点が側壁部１１ａとコーナー部１１ｂの境界である。さらに、ルツボの底の曲率が一定の部分が底部１１ｃであり、ルツボの底の中心からの距離が増したときに曲率が変化し始める点が底部１１ｃとコーナー部１１ｂとの境界である。 The silica glass crucible 11 includes a cylindrical side wall part 11a, a curved bottom part 11c, and a corner part 11b that connects the side wall part 11a and the bottom part 11c and has a larger curvature than the bottom part 11c. In the present invention, the corner portion 11b is a portion connecting the side wall portion 11a and the bottom portion 11c, from a point where the tangent line of the corner portion curve overlaps the side wall portion 11a of the silica glass crucible to a point having a common tangent line with the bottom portion 11c. Means the part. In other words, the point where the side wall portion 11a of the silica glass crucible 11 begins to bend is the boundary between the side wall portion 11a and the corner portion 11b. Further, the portion where the curvature of the bottom of the crucible is constant is the bottom portion 11c, and the point where the curvature starts to change when the distance from the center of the bottom of the crucible increases is the boundary between the bottom portion 11c and the corner portion 11b.
＜２．多結晶シリコンの充填及び熔融＞
シリコン単結晶の引き上げ時には、ルツボ１１内に多結晶シリコンを充填し、この状態でルツボ１の周囲に配置されたカーボンヒーターで多結晶シリコンを加熱して熔融させて、図１（ａ）に示すように、シリコン融液２３を得る。
<2. Filling and melting of polycrystalline silicon>
When pulling up the silicon single crystal, the crucible 11 is filled with polycrystalline silicon, and in this state, the polycrystalline silicon is heated and melted with a carbon heater disposed around the crucible 1, as shown in FIG. Thus, the silicon melt 23 is obtained.
シリコン融液２３の体積は、多結晶シリコン２１の質量によって定まるので、シリコン融液２３の液面２３ａの初期の高さ位置Ｈ０は、多結晶シリコン２１の質量とルツボ１１の内表面の三次元形状によって決まる。本発明によれば、後述する方法によって、ルツボ１１の内表面の三次元形状が定まるので、ルツボ１１の任意の高さ位置までの容積が特定され、従って、シリコン融液２３液面２３ａの初期の高さ位置Ｈ０が決定される。 Since the volume of the silicon melt 23 is determined by the mass of the polycrystalline silicon 21, the initial height position H 0 of the liquid surface 23 a of the silicon melt 23 is three-dimensional between the mass of the polycrystalline silicon 21 and the inner surface of the crucible 11. It depends on the shape. According to the present invention, since the three-dimensional shape of the inner surface of the crucible 11 is determined by the method described later, the volume up to an arbitrary height position of the crucible 11 is specified, and accordingly, the initial level of the silicon melt 23 liquid surface 23a is specified. The height position H0 is determined.
シリコン融液２３の液面２３ａの初期の高さ位置Ｈ０が決定された後は、図１（ａ）に示すように、種結晶２４の先端を高さ位置Ｈ０まで下降させてシリコン融液２３に接触させ、その後、ゆっくりと引き上げることによって、シリコン単結晶２５の引き上げを行う。 After the initial height position H0 of the liquid surface 23a of the silicon melt 23 is determined, the tip of the seed crystal 24 is lowered to the height position H0 as shown in FIG. Then, the silicon single crystal 25 is pulled up by slowly pulling it up.
図１（ｂ）に示すように、シリコン単結晶２５の直胴部（直径が一定の部位）を引き上げているときに、液面２３ａがルツボ１１の側壁部１１ａに位置している場合には、一定の速度で引き上げると液面２３ａの降下速度Ｖはほぼ一定になるので、引き上げの制御は容易である。 As shown in FIG. 1 (b), when the liquid body 23 a is positioned on the side wall 11 a of the crucible 11 when the straight body part (part having a constant diameter) of the silicon single crystal 25 is pulled up. If the liquid surface 23a is pulled up at a constant speed, the descent speed V of the liquid surface 23a becomes almost constant, so that the pulling up control is easy.
しかし、図１（ｃ）に示すように、液面２３ａがルツボ１１のコーナー部１１ｂに到達すると、液面２３ａの下降に伴ってその面積が急激に縮小するので、液面２３ａの降下速度Ｖが急激に大きくなる。降下速度Ｖは、コーナー部１１ｂの内表面形状に依存しているが、この内表面形状がルツボ毎に若干異なっているので、降下速度Ｖがどのように変化するのかを事前に把握することは困難であり、引き上げの自動化の妨げになっていた。 However, as shown in FIG. 1 (c), when the liquid level 23a reaches the corner 11b of the crucible 11, the area rapidly decreases as the liquid level 23a descends. Increases rapidly. The descending speed V depends on the inner surface shape of the corner portion 11b. However, since the inner surface shape is slightly different for each crucible, it is impossible to grasp in advance how the descending speed V changes. It was difficult and hindered automated lifting.
本実施形態では、後述する方法によって、ルツボの内表面の三次元形状を正確に測定するので、コーナー部１１ｂの内表面形状が事前に分かり、従って、降下速度Ｖがどのように変化するのかを正確に予測することができるので、その予測に基づいて、シリコン単結晶２５の引き上げ速度等の引き上げ条件を決定することにより、コーナー部１１ｂにおいても有転移化を防止し且つ引き上げを自動化することが可能である。 In the present embodiment, since the three-dimensional shape of the inner surface of the crucible is accurately measured by a method described later, the inner surface shape of the corner portion 11b is known in advance, and therefore, how the descent speed V changes. Since the prediction can be performed accurately, by determining the pulling conditions such as the pulling speed of the silicon single crystal 25 based on the prediction, it is possible to prevent the transition from occurring in the corner portion 11b and to automate the pulling. Is possible.
＜３．ルツボの内表面の三次元形状の測定方法＞
以下、図２〜図５を用いて、ルツボの内表面の三次元形状の測定方法について説明する。本実施形態では、レーザー変位計などからなる内部測距部１７をルツボ内表面に沿って非接触で移動させ、移動経路上の複数の測定点において、ルツボ内表面に対してレーザー光を斜め方向に照射し、その反射光を検出することによって、ルツボの内表面の三次元形状を測定する。以下、詳細に説明する。また、内表面形状を測定する際に、透明層１３と気泡含有層１５の界面の三次元形状も同時に測定することができ、また、内部測距部１９を用いることによってルツボの外表面の三次元形状も測定することができるので、これらの点についても合わせて説明する。
<3. Method for measuring the 3D shape of the inner surface of the crucible>
Hereinafter, a method for measuring the three-dimensional shape of the inner surface of the crucible will be described with reference to FIGS. In the present embodiment, the internal distance measuring unit 17 including a laser displacement meter is moved in a non-contact manner along the inner surface of the crucible, and laser light is obliquely directed to the inner surface of the crucible at a plurality of measurement points on the movement path. And measuring the three-dimensional shape of the inner surface of the crucible by detecting the reflected light. Details will be described below. Further, when measuring the inner surface shape, the three-dimensional shape of the interface between the transparent layer 13 and the bubble-containing layer 15 can also be measured at the same time. Since the original shape can also be measured, these points will be described together.
＜３−１．シリカガラスルツボの設置、内部ロボットアーム、内部測距部＞
測定対象であるシリカガラスルツボ１１は、開口部が下向きになるように回転可能な回転台９上に載置されている。ルツボ１１に覆われる位置に設けられた基台１上には、内部ロボットアーム５が設置されている。内部ロボットアーム５は、複数のアーム５ａと、これらのアーム５ａを回転可能に支持する複数のジョイント５ｂと、本体部５ｃを備える。本体部５ｃには図示しない外部端子が設けられており、外部とのデータ交換が可能になっている。内部ロボットアーム５の先端にはルツボ１１の内表面形状の測定を行う内部測距部１７が設けられている。内部測距部１７は、ルツボ１１の内表面に対してレーザー光を照射し、内表面からの反射光を検出することによって内部測距部１７からルツボ１１の内表面までの距離を測定する。本体部５ｃ内には、ジョイント５ｂ及び内部測距部１７の制御を行う制御部が設けられている。制御部は、本体部５ｃ設けられたプログラム又は外部入力信号に基づいてジョイント５ｂを回転させてアーム５を動かすことによって、内部測距部１７を任意の三次元位置に移動させる。具体的には、内部測距部１７をルツボ内表面に沿って非接触で移動させる。従って、制御部には、ルツボ内表面の大まかな形状データを与え、そのデータに従って、内部測距部１７の位置を移動させる。より具体的には、例えば、図２（ａ）に示すようなルツボ１１の開口部近傍に近い位置から測定を開始し、図２（ｂ）に示すように、ルツボ１１の底部１１ｃに向かって内部測距部１７を移動させ、移動経路上の複数の測定点において測定を行う。測定間隔は、例えば、１〜５ｍｍであり、例えば２ｍｍである。測定は、予め内部測距部１７内に記憶されたタイミングで行うか、又は外部トリガに従って行う。測定結果は、内部測距部１７内の記憶部に格納されて、測定終了後にまとめて本体部５ｃに送られるか、又は測定の度に、逐次本体部５ｃに送られるようにする。内部測距部１７は、本体部５ｃとは別に設けられた制御部によって制御するように構成してもよい。
<3-1. Installation of silica glass crucible, internal robot arm, internal distance measuring section>
The silica glass crucible 11 to be measured is placed on a turntable 9 that can be rotated so that the opening is directed downward. On the base 1 provided at a position covered with the crucible 11, an internal robot arm 5 is installed. The internal robot arm 5 includes a plurality of arms 5a, a plurality of joints 5b that rotatably support these arms 5a, and a main body 5c. The main body 5c is provided with an external terminal (not shown) so that data exchange with the outside is possible. An internal distance measuring unit 17 for measuring the inner surface shape of the crucible 11 is provided at the tip of the internal robot arm 5. The internal distance measuring unit 17 measures the distance from the internal distance measuring unit 17 to the inner surface of the crucible 11 by irradiating the inner surface of the crucible 11 with laser light and detecting reflected light from the inner surface. A control unit that controls the joint 5b and the internal distance measuring unit 17 is provided in the main body 5c. The control unit moves the internal distance measuring unit 17 to an arbitrary three-dimensional position by rotating the joint 5b and moving the arm 5 based on a program provided in the main body 5c or an external input signal. Specifically, the internal distance measuring unit 17 is moved in a non-contact manner along the inner surface of the crucible. Therefore, rough shape data of the inner surface of the crucible is given to the control unit, and the position of the internal distance measuring unit 17 is moved according to the data. More specifically, for example, the measurement is started from a position close to the vicinity of the opening of the crucible 11 as shown in FIG. 2A, and toward the bottom 11c of the crucible 11 as shown in FIG. The internal distance measuring unit 17 is moved to perform measurement at a plurality of measurement points on the movement path. The measurement interval is, for example, 1 to 5 mm, for example, 2 mm. The measurement is performed at a timing stored in the internal distance measuring unit 17 in advance or according to an external trigger. The measurement results are stored in the storage unit in the internal distance measuring unit 17, and are sent to the main body unit 5c collectively after the measurement is completed, or are sequentially sent to the main body unit 5c for each measurement. The internal distance measuring unit 17 may be configured to be controlled by a control unit provided separately from the main body 5c.
ルツボの開口部から底部１１ｃまでの測定が終わると、回転台９を少し回転させ、同様の測定行う。この測定は、底部１１ｃから開口部に向かって行ってもよい。回転台９の回転角は、精度と測定時間との考慮して決定されるが、例えば、２〜１０度である。回転角が大きすぎると測定精度が十分でなく、小さすぎると測定時間が掛かりすぎる。回転台９の回転は、内蔵プログラム又は外部入力信号に基づいて制御される。回転台９の回転角は、ロータリーエンコーダ等によって検出可能である。回転台９の回転は、内部測距部１７及び後述する外部測距部１９の移動と連動してすることが好ましく、これによって、内部測距部１７及び外部測距部１９の３次元座標の算出が容易になる。 When the measurement from the opening of the crucible to the bottom 11c is completed, the turntable 9 is slightly rotated and the same measurement is performed. This measurement may be performed from the bottom 11c toward the opening. The rotation angle of the turntable 9 is determined in consideration of accuracy and measurement time, and is, for example, 2 to 10 degrees. If the rotation angle is too large, the measurement accuracy is not sufficient, and if it is too small, it takes too much measurement time. The rotation of the turntable 9 is controlled based on a built-in program or an external input signal. The rotation angle of the turntable 9 can be detected by a rotary encoder or the like. It is preferable that the rotation of the turntable 9 be interlocked with the movement of the internal distance measuring unit 17 and the external distance measuring unit 19 which will be described later, whereby the three-dimensional coordinates of the internal distance measuring unit 17 and the external distance measuring unit 19 are changed. Calculation becomes easy.
後述するが、内部測距部１７は、内部測距部１７から内表面までの距離（内表面距離）、及び内部測距部１７から透明層１３と気泡含有層１５の界面までの距離（界面距離）の両方を測定することができる。ジョイント５ｂの角度はジョイント５ｂに設けられたロータリーエンコーダ等によって既知であるので、各測定点での内部測距部１７の位置の三次元座標及び方向が既知になるので、内表面距離及び界面距離が求まれば、内表面での三次元座標、及び界面での三次元座標が既知となる。そして、ルツボ１１の開口部から底部１１ｃまでの測定が、ルツボ１１の全周に渡って行われるので、ルツボ１１の内表面の三次元形状、及び界面の三次元形状が既知になる。また、内表面と界面の間の距離が既知になるので、透明層１３の厚さも既知になり、透明層の厚さの三次元分布が求められる。 As will be described later, the internal distance measuring unit 17 includes a distance from the internal distance measuring unit 17 to the inner surface (inner surface distance) and a distance from the inner distance measuring unit 17 to the interface between the transparent layer 13 and the bubble-containing layer 15 (interface). Both distances can be measured. Since the angle of the joint 5b is known by a rotary encoder or the like provided in the joint 5b, the three-dimensional coordinates and direction of the position of the internal distance measuring unit 17 at each measurement point are known. Is obtained, the three-dimensional coordinates on the inner surface and the three-dimensional coordinates on the interface are known. And since the measurement from the opening part of the crucible 11 to the bottom part 11c is performed over the perimeter of the crucible 11, the three-dimensional shape of the inner surface of the crucible 11 and the three-dimensional shape of the interface become known. Further, since the distance between the inner surface and the interface is known, the thickness of the transparent layer 13 is also known, and a three-dimensional distribution of the thickness of the transparent layer is obtained.
＜３−２．外部ロボットアーム、外部測距部＞
ルツボ１１の外部に設けられた基台３上には、外部ロボットアーム７が設置されている。外部ロボットアーム７は、複数のアーム７ａと、これらのアームを回転可能に支持する複数のジョイント７ｂと、本体部７ｃを備える。本体部７ｃには図示しない外部端子が設けられており、外部とのデータ交換が可能になっている。外部ロボットアーム７の先端にはルツボ１１の外表面形状の測定を行う外部測距部１９が設けられている。外部測距部１９は、ルツボ１１の外表面に対してレーザー光を照射し、外表面からの反射光を検出することによって外部測距部１９からルツボ１１の外表面までの距離を測定する。本体部７ｃ内には、ジョイント７ｂ及び外部測距部１９の制御を行う制御部が設けられている。制御部は、本体部７ｃ設けられたプログラム又は外部入力信号に基づいてジョイント７ｂを回転させてアーム７を動かすことによって、外部測距部１９を任意の三次元位置に移動させる。具体的には、外部測距部１９をルツボ外表面に沿って非接触で移動させる。従って、制御部には、ルツボ外表面の大まかな形状データを与え、そのデータに従って、外部測距部１９の位置を移動させる。より具体的には、例えば、図２（ａ）に示すようなルツボ１１の開口部近傍に近い位置から測定を開始し、図２（ｂ）に示すように、ルツボ１１の底部１１ｃに向かって外部測距部１９を移動させ、移動経路上の複数の測定点において測定を行う。測定間隔は、例えば、１〜５ｍｍであり、例えば２ｍｍである。測定は、予め外部測距部１９内に記憶されたタイミングで行うか、又は外部トリガに従って行う。測定結果は、外部測距分１９内の記憶部に格納されて、測定終了後にまとめて本体部７ｃに送られるか、又は測定の度に、逐次本体部７ｃに送られるようにする。外部測距部１９は、本体部７ｃとは別に設けられた制御部によって制御するように構成してもよい。
<3-2. External robot arm, external distance measuring unit>
An external robot arm 7 is installed on a base 3 provided outside the crucible 11. The external robot arm 7 includes a plurality of arms 7a, a plurality of joints 7b that rotatably support these arms, and a main body portion 7c. The main body 7c is provided with an external terminal (not shown) so that data exchange with the outside is possible. An external distance measuring unit 19 that measures the outer surface shape of the crucible 11 is provided at the tip of the external robot arm 7. The external distance measuring unit 19 measures the distance from the external distance measuring unit 19 to the outer surface of the crucible 11 by irradiating the outer surface of the crucible 11 with laser light and detecting the reflected light from the outer surface. A control unit that controls the joint 7b and the external distance measuring unit 19 is provided in the main body 7c. The control unit moves the external distance measuring unit 19 to an arbitrary three-dimensional position by rotating the joint 7b and moving the arm 7 based on a program provided in the main body unit 7c or an external input signal. Specifically, the external distance measuring unit 19 is moved in a non-contact manner along the outer surface of the crucible. Therefore, rough shape data of the outer surface of the crucible is given to the control unit, and the position of the external distance measuring unit 19 is moved according to the data. More specifically, for example, the measurement is started from a position close to the vicinity of the opening of the crucible 11 as shown in FIG. 2A, and toward the bottom 11c of the crucible 11 as shown in FIG. The external distance measuring unit 19 is moved to perform measurement at a plurality of measurement points on the movement path. The measurement interval is, for example, 1 to 5 mm, for example, 2 mm. The measurement is performed at a timing stored in advance in the external distance measuring unit 19 or according to an external trigger. The measurement results are stored in the storage unit in the external distance measuring unit 19 and are collectively sent to the main unit 7c after the measurement is completed, or are sequentially sent to the main unit 7c every measurement. The external distance measuring unit 19 may be configured to be controlled by a control unit provided separately from the main body unit 7c.
内部測距部１７と外部測距部１９は、同期させて移動させてもよいが、内表面形状の測定と外表面形状の測定は独立して行われるので、必ずしも同期させる必要はない。 The internal distance measuring unit 17 and the external distance measuring unit 19 may be moved in synchronization. However, since the measurement of the inner surface shape and the measurement of the outer surface shape are performed independently, it is not always necessary to synchronize.
外部測距部１９は、外部測距部１９から外表面までの距離（外表面距離）を測定することができる。ジョイント７ｂの角度はジョイント７ｂに設けられたロータリーエンコーダ等によって既知であるので、外部測距部１９の位置の三次元座標及び方向が既知になるので、外表面距離が求まれば、外表面での三次元座標が既知となる。そして、ルツボ１１の開口部から底部１１ｃまでの測定が、ルツボ１１の全周に渡って行われるので、ルツボ１１の外表面の三次元形状が既知になる。
以上より、ルツボの内表面及び外表面の三次元形状が既知になるので、ルツボの壁厚の三次元分布が求められる。
The external distance measuring unit 19 can measure the distance (outer surface distance) from the external distance measuring unit 19 to the outer surface. Since the angle of the joint 7b is known by a rotary encoder or the like provided in the joint 7b, the three-dimensional coordinates and direction of the position of the external distance measuring unit 19 are known. The three-dimensional coordinates are known. And since the measurement from the opening part of the crucible 11 to the bottom part 11c is performed over the perimeter of the crucible 11, the three-dimensional shape of the outer surface of the crucible 11 becomes known.
From the above, since the three-dimensional shape of the inner surface and the outer surface of the crucible becomes known, a three-dimensional distribution of the wall thickness of the crucible is obtained.
＜３−３．距離測定の詳細＞
次に、図３を用いて、内部測距部１７及び外部測距部１９による距離測定の詳細を説明する。
図３に示すように、内部測距部１７は、ルツボ１１の内表面側（透明層１３側）に配置され、外部測距部１９は、ルツボ１１の外表面側（気泡含有層１５側）に配置される。内部測距部１７は、出射部１７ａ及び検出部１７ｂを備える。外部測距部１９は、出射部１９ａ及び検出部１９ｂを備える。また、内部測距部１７及び外部測距部１９は、図示しない制御部及び外部端子を備える。出射部１７ａ及び１９ａは、レーザー光を出射するものであり、例えば、半導体レーザーを備えるものである。出射されるレーザー光の波長は、特に限定されないが、例えば、波長６００〜７００ｎｍの赤色レーザー光である。検出部１７ｂ及び１９ｂは、例えばＣＣＤで構成され、光が当たった位置に基づいて三角測量法の原理に基づいてターゲットまでの距離が決定される。
<3-3. Details of distance measurement>
Next, details of distance measurement by the internal distance measuring unit 17 and the external distance measuring unit 19 will be described with reference to FIG.
As shown in FIG. 3, the internal distance measuring unit 17 is arranged on the inner surface side (transparent layer 13 side) of the crucible 11, and the external distance measuring unit 19 is arranged on the outer surface side (bubble containing layer 15 side) of the crucible 11. Placed in. The internal distance measuring unit 17 includes an emitting unit 17a and a detecting unit 17b. The external distance measuring unit 19 includes an emitting unit 19a and a detecting unit 19b. The internal distance measuring unit 17 and the external distance measuring unit 19 include a control unit and an external terminal (not shown). The emitting portions 17a and 19a emit laser light, and include, for example, a semiconductor laser. The wavelength of the emitted laser light is not particularly limited, but is, for example, red laser light having a wavelength of 600 to 700 nm. The detectors 17b and 19b are composed of, for example, a CCD, and the distance to the target is determined based on the principle of triangulation based on the position where the light hits.
内部測距部１７の出射部１７ａから出射されたレーザー光は、一部が内表面（透明層１３の表面）で反射し、一部が透明層１３と気泡含有層１５の界面で反射し、これらの反射光（内表面反射光、界面反射光）が検出部１７ｂに当たって検出される。図３から明らかなように、内表面反射光と界面反射光は、検出部１７ｂの異なる位置に当たっており、この位置の違いによって、内部測距部１７から内表面までの距離（内表面距離）及び界面までの距離（界面距離）がそれぞれ決定される。好適な入射角θは、内表面の状態、透明層１３の厚さ、気泡含有層１５の状態等によって、変化しうるが例えば３０〜６０度である。 A part of the laser light emitted from the emitting part 17a of the internal distance measuring part 17 is reflected by the inner surface (the surface of the transparent layer 13), and partly reflected by the interface between the transparent layer 13 and the bubble-containing layer 15, These reflected lights (inner surface reflected light and interface reflected light) strike the detection unit 17b and are detected. As is clear from FIG. 3, the inner surface reflected light and the interface reflected light hit different positions of the detection unit 17b, and due to the difference in position, the distance from the inner distance measuring unit 17 to the inner surface (inner surface distance) and The distance to the interface (interface distance) is determined. A suitable incident angle θ may vary depending on the state of the inner surface, the thickness of the transparent layer 13, the state of the bubble-containing layer 15, etc., but is, for example, 30 to 60 degrees.
図４は、市販のレーザー変位計を用いて測定された実際の測定結果を示す。図４に示すように、２つのピークが観察されており、内表面側のピークが内表面反射光によるピークであり、外表面側のピークが界面反射光によるピークに対応する。このように、透明層１３と気泡含有層１５の界面からの反射光によるピークもクリアに検出されている。従来は、このような方法で界面の特定がなされたことがなく、この結果は非常に斬新である。 FIG. 4 shows the actual measurement results measured using a commercially available laser displacement meter. As shown in FIG. 4, two peaks are observed, the peak on the inner surface side corresponds to the peak due to the inner surface reflected light, and the peak on the outer surface side corresponds to the peak due to the interface reflected light. Thus, the peak due to the reflected light from the interface between the transparent layer 13 and the bubble-containing layer 15 is also clearly detected. Conventionally, the interface has not been specified in this way, and this result is very novel.
内部測距部１７から内表面までの距離が遠すぎる場合や、内表面又は界面が局所的に傾いている場合には、２つのピークが観測されない場合がある。その場合には、内部測距部１７を内表面に近づけたり、内部測距部１７の傾けてレーザー光の出射方向を変化させて、２つのピークが観測される位置及び角度を探索することが好ましい。また、２つのピークが同時に観測されなくても、ある位置及び角度において内表面反射光によるピークを観測し、別の位置及び角度において界面反射光によるピークを観測するようにしてもよい。また、内部測距部１７が内表面に接触することを避けるために、最大近接位置を設定しておいて、ピークが観測されない場合でも、その位置よりも内表面に近づけないようにすることが好ましい。
また、透明層１３中に独立した気泡が存在する場合、この気泡からの反射光を内部測距部１７が検出してしまい、透明層１３と気泡含有層１５の界面を適切に検出できない場合がある。従って、ある測定点Ａで測定された界面の位置が前後の測定点で測定された界面の位置から大きく（所定の基準値を超えて）ずれている場合には、測定点Ａでのデータを除外してもよい。また、その場合、測定点Ａからわずかにずれた位置で再度測定を行って、得られたデータを採用してもよい。
If the distance from the internal distance measuring unit 17 to the inner surface is too far, or if the inner surface or interface is locally inclined, two peaks may not be observed. In this case, the position and angle at which two peaks are observed can be searched by moving the internal distance measuring unit 17 closer to the inner surface or by tilting the internal distance measuring unit 17 to change the laser beam emission direction. preferable. Further, even if the two peaks are not observed simultaneously, the peak due to the inner surface reflected light may be observed at a certain position and angle, and the peak due to the interface reflected light may be observed at another position and angle. In order to prevent the internal distance measuring unit 17 from coming into contact with the inner surface, a maximum proximity position is set so that even if no peak is observed, the inner distance measuring unit 17 cannot be closer to the inner surface than that position. preferable.
In addition, when there are independent bubbles in the transparent layer 13, the internal distance measuring unit 17 may detect the reflected light from the bubbles, and the interface between the transparent layer 13 and the bubble-containing layer 15 may not be detected properly. is there. Therefore, when the position of the interface measured at a certain measurement point A is greatly deviated (exceeding a predetermined reference value) from the position of the interface measured at the preceding and following measurement points, the data at the measurement point A is It may be excluded. In that case, data obtained by performing measurement again at a position slightly deviated from the measurement point A may be employed.
また、外部測距部１９の出射部１９ａから出射されたレーザー光は、外表面（気泡含有層１５）の表面で反射し、その反射光（外表面反射光）が検出部１９ｂに当たって検出され、検出部１９ｂ上での検出位置に基づいて外部測距部１９と外表面の間の距離が決定される。図５は、市販のレーザー変位計を用いて測定された実際の測定結果を示す。図５に示すように、１つのピークのみが観察される。ピークが観測されない場合には、外部測距部１９を内表面に近づけたり、外部測距部１９の傾けてレーザー光の出射方向を変化させて、ピークが観測される位置及び角度を探索することが好ましい。 The laser light emitted from the emitting portion 19a of the external distance measuring section 19 is reflected by the surface of the outer surface (bubble-containing layer 15), and the reflected light (outer surface reflected light) strikes the detecting portion 19b and is detected. The distance between the external distance measuring unit 19 and the outer surface is determined based on the detection position on the detection unit 19b. FIG. 5 shows the actual measurement results measured using a commercially available laser displacement meter. As shown in FIG. 5, only one peak is observed. When the peak is not observed, the external distance measuring unit 19 is brought closer to the inner surface, or the external distance measuring unit 19 is tilted to change the emission direction of the laser light to search for the position and angle at which the peak is observed. Is preferred.
Claims (3)
前記シリコン融液の液面が前記コーナー部に到達した後の前記シリコン単結晶の引き上げ条件が、前記シリカガラスルツボの内表面の三次元形状に基づいて決定され、
前記内表面の表面粗さの三次元分布は、
前記シリカガラスルツボの内表面に沿って非接触で内部測距部を移動させ、
移動経路上の複数の測定点において、内部測距部から前記シリカガラスルツボの内表面に対して斜め方向にレーザー光を照射し、前記内表面からの内表面反射光を検出することによって、内部測距部と前記内表面の間の内表面距離を測定し、
各測定点の三次元座標と、前記内表面距離を関連付けることによって、前記シリカガラスルツボの内表面の三次元形状を求める工程を備える方法によって決定される、シリコン単結晶の製造方法。 A silicon single crystal is pulled up from a silicon melt held in a silica glass crucible having a cylindrical side wall portion, a curved bottom portion, and a corner portion connecting the side wall portion and the bottom portion and having a larger curvature than the bottom portion. With a process,
The pulling condition of the silicon single crystal after the liquid level of the silicon melt reaches the corner is determined based on the three-dimensional shape of the inner surface of the silica glass crucible,
The three-dimensional distribution of the surface roughness of the inner surface is
Move the internal distance measuring unit in a non-contact manner along the inner surface of the silica glass crucible,
By irradiating laser light obliquely to the inner surface of the silica glass crucible from the internal distance measuring unit at a plurality of measurement points on the moving path, and detecting the inner surface reflected light from the inner surface, Measure the inner surface distance between the distance measuring unit and the inner surface,
A method for producing a silicon single crystal, comprising: determining a three-dimensional shape of an inner surface of the silica glass crucible by associating a three-dimensional coordinate of each measurement point with the inner surface distance.
前記シリカガラスルツボは、内部ロボットアームを覆うように配置される、請求項１又は２に記載の方法。 The internal ranging unit is fixed to an internal robot arm configured to be able to move the internal ranging unit three-dimensionally,
The method according to claim 1 or 2, wherein the silica glass crucible is arranged to cover an internal robot arm.
Priority Applications (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011282412A JP5739797B2 (en) | 2011-12-22 | 2011-12-22 | Method for producing silicon single crystal |
| KR1020147020091A KR101638584B1 (en) | 2011-12-22 | 2012-10-31 | Method for evaluating silica glass crucible, method for producing silicon single crystals |
| US14/365,523 US9809902B2 (en) | 2011-12-22 | 2012-10-31 | Method for evaluating silica glass crucible, method for producing silicon single crystals |
| EP12859405.8A EP2796595B1 (en) | 2011-12-22 | 2012-10-31 | Method for evaluating silica glass crucible, method for producing silicon single crystals |
| CN201280063279.7A CN104145051B (en) | 2011-12-22 | 2012-10-31 | The evaluation method of silica glass crucible, the manufacturing method of monocrystalline silicon |
| PCT/JP2012/078260 WO2013094318A1 (en) | 2011-12-22 | 2012-10-31 | Method for evaluating silica glass crucible, method for producing silicon single crystals |
| TW101140627A TWI480505B (en) | 2011-12-22 | 2012-11-01 | Evaluation method of silica glass crucible and manufacture method of silicon single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011282412A JP5739797B2 (en) | 2011-12-22 | 2011-12-22 | Method for producing silicon single crystal |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2015089367A Division JP5978343B2 (en) | 2015-04-24 | 2015-04-24 | Method for producing silicon single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2013133230A true JP2013133230A (en) | 2013-07-08 |
| JP5739797B2 JP5739797B2 (en) | 2015-06-24 |
Family
ID=48910184
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2011282412A Active JP5739797B2 (en) | 2011-12-22 | 2011-12-22 | Method for producing silicon single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP5739797B2 (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08278117A (en) * | 1995-02-06 | 1996-10-22 | Mitsubishi Materials Corp | Attitude control device for work apparatus relative to work object plane, crucible instrumentation device with the control device and painting device |
| JPH09196646A (en) * | 1996-01-23 | 1997-07-31 | Nippon Telegr & Teleph Corp <Ntt> | Method and apparatus for measuring surface nature |
| JPH10185545A (en) * | 1996-12-27 | 1998-07-14 | Shinetsu Eng Kk | Shape measuring instrument for quartz crucible |
| JP2001048693A (en) * | 1999-08-06 | 2001-02-20 | Hitachi Chem Co Ltd | Glassy carbon crucible having inner face being polygonal form |
| JP2004271247A (en) * | 2003-03-06 | 2004-09-30 | Japan Siper Quarts Corp | Glass layer thickness measuring method and measuring device |
| JP2006096618A (en) * | 2004-09-29 | 2006-04-13 | Toshiba Ceramics Co Ltd | Apparatus for removing object to be removed in quartz glass crucible |
-
2011
- 2011-12-22 JP JP2011282412A patent/JP5739797B2/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08278117A (en) * | 1995-02-06 | 1996-10-22 | Mitsubishi Materials Corp | Attitude control device for work apparatus relative to work object plane, crucible instrumentation device with the control device and painting device |
| JPH09196646A (en) * | 1996-01-23 | 1997-07-31 | Nippon Telegr & Teleph Corp <Ntt> | Method and apparatus for measuring surface nature |
| JPH10185545A (en) * | 1996-12-27 | 1998-07-14 | Shinetsu Eng Kk | Shape measuring instrument for quartz crucible |
| JP2001048693A (en) * | 1999-08-06 | 2001-02-20 | Hitachi Chem Co Ltd | Glassy carbon crucible having inner face being polygonal form |
| JP2004271247A (en) * | 2003-03-06 | 2004-09-30 | Japan Siper Quarts Corp | Glass layer thickness measuring method and measuring device |
| JP2006096618A (en) * | 2004-09-29 | 2006-04-13 | Toshiba Ceramics Co Ltd | Apparatus for removing object to be removed in quartz glass crucible |
Also Published As
| Publication number | Publication date |
|---|---|
| JP5739797B2 (en) | 2015-06-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101623178B1 (en) | Device for assisting with setting of manufacturing conditions for silica glass crucible, device for assisting with setting of manufacturing conditions for mold for manufacturing silica glass crucible, device for assisting with condition setting for raising monocrystalline silicon using silica glass crucible | |
| JP5749151B2 (en) | Method for measuring the three-dimensional shape of the Raman spectrum of silica glass crucibles | |
| JP6123001B2 (en) | Method for evaluating silica glass crucible, method for producing silicon single crystal | |
| JP6162867B2 (en) | Method for producing silicon single crystal | |
| JP6162848B2 (en) | Method for producing silicon single crystal | |
| JP5978343B2 (en) | Method for producing silicon single crystal | |
| JP5709737B2 (en) | Method for producing silicon single crystal | |
| JP5739797B2 (en) | Method for producing silicon single crystal | |
| JP5749149B2 (en) | Method for measuring three-dimensional shape of silica glass crucible | |
| JP2017160123A (en) | Production method of silicon single crystal | |
| JP5682553B2 (en) | A device that supports the setting of silicon single crystal pulling conditions using a silica glass crucible. | |
| JP5818675B2 (en) | Method for determining three-dimensional distribution of bubble distribution in silica glass crucible, method for producing silicon single crystal | |
| JP5925348B2 (en) | Method for producing silicon single crystal | |
| JP2017154971A (en) | Method of manufacturing silicon single crystal | |
| JP5946561B2 (en) | Method for determining three-dimensional distribution of surface roughness of silica glass crucible, method for producing silicon single crystal | |
| JP6162870B2 (en) | Method for producing silica glass crucible | |
| JP5996718B2 (en) | Method for measuring three-dimensional shape of silica glass crucible, method for producing silicon single crystal | |
| JP5749152B2 (en) | Method for measuring three-dimensional shape of surface roughness of silica glass crucible | |
| JP5946560B2 (en) | Method for determining three-dimensional distribution of Raman spectrum of silica glass crucible, method for producing silicon single crystal | |
| JP6123000B2 (en) | Method for evaluating silica glass crucible, method for producing silicon single crystal | |
| JP5923644B2 (en) | Method for determining three-dimensional distribution of infrared absorption spectrum of silica glass crucible, method for producing silicon single crystal | |
| JP6162847B2 (en) | Method for determining three-dimensional distribution of infrared absorption spectrum of silica glass crucible and method for producing silicon single crystal | |
| JP5749150B2 (en) | Method for determining three-dimensional distribution of infrared absorption spectrum of silica glass crucible, method for producing silicon single crystal | |
| JP6114795B2 (en) | Method for determining three-dimensional distribution of bubble distribution in silica glass crucible, method for producing silicon single crystal | |
| JP2017215325A (en) | Measuring method of silica glass crucible |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20131213 |
|
| A711 | Notification of change in applicant |
Free format text: JAPANESE INTERMEDIATE CODE: A712 Effective date: 20131213 |
|
| RD04 | Notification of resignation of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7424 Effective date: 20141027 |
|
| RD02 | Notification of acceptance of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7422 Effective date: 20141121 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20150116 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20150317 |
|
| 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: 20150408 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20150424 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 5739797 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |