JP2814036B2 - Apparatus and method for determining use limit of graphite crucible - Google Patents
Apparatus and method for determining use limit of graphite crucibleInfo
- Publication number
- JP2814036B2 JP2814036B2 JP15140592A JP15140592A JP2814036B2 JP 2814036 B2 JP2814036 B2 JP 2814036B2 JP 15140592 A JP15140592 A JP 15140592A JP 15140592 A JP15140592 A JP 15140592A JP 2814036 B2 JP2814036 B2 JP 2814036B2
- Authority
- JP
- Japan
- Prior art keywords
- graphite crucible
- heavy metal
- metal vapor
- use limit
- concentration
- 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.)
- Expired - Lifetime
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 56
- 229910002804 graphite Inorganic materials 0.000 title claims description 56
- 239000010439 graphite Substances 0.000 title claims description 56
- 238000000034 method Methods 0.000 title claims description 19
- 229910001385 heavy metal Inorganic materials 0.000 claims description 46
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 23
- 239000013078 crystal Substances 0.000 claims description 23
- 229910052710 silicon Inorganic materials 0.000 claims description 23
- 239000010703 silicon Substances 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000007547 defect Effects 0.000 description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 14
- 239000001301 oxygen Substances 0.000 description 14
- 229910052760 oxygen Inorganic materials 0.000 description 14
- 239000010453 quartz Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 5
- 238000011109 contamination Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、黒鉛るつぼの使用限度
判定装置および判定方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus and a method for determining the limit of use of a graphite crucible.
【０００２】[0002]
【従来の技術】半導体集積回路の基本材料であるシリコ
ン単結晶の製造方法の一つとして、るつぼ内の原料融液
から円柱状の単結晶を引き上げるＣＺ法が用いられてい
る。ＣＺ法においては、チャンバ内に石英、黒鉛等から
なるるつぼを設け、このるつぼに収容した多結晶シリコ
ン等の原料をるつぼの外周に設けたヒータによって加熱
溶融した後、シード軸に取り付けた種子結晶を前記融液
に浸漬し、シード軸を回転しつつ上方に引き上げて単結
晶を成長させている。前記るつぼは一般に、黒鉛るつぼ
内に石英るつぼが嵌着されていて、二重構造となってい
る。そして、石英るつぼは１回のシリコン単結晶引き上
げが完了すると、そのつど新品と交換するが、黒鉛るつ
ぼは特別な理由がない限り連続して使用している。2. Description of the Related Art As one method of manufacturing a silicon single crystal, which is a basic material of a semiconductor integrated circuit, a CZ method of pulling a columnar single crystal from a raw material melt in a crucible is used. In the CZ method, a crucible made of quartz, graphite, or the like is provided in a chamber, and a material such as polycrystalline silicon contained in the crucible is heated and melted by a heater provided on the outer periphery of the crucible, and then the seed crystal attached to a seed shaft is provided. Is immersed in the melt and pulled upward while rotating the seed shaft to grow a single crystal. The crucible generally has a double structure in which a quartz crucible is fitted in a graphite crucible. The quartz crucible is replaced with a new one each time the silicon single crystal is pulled up once, but the graphite crucible is continuously used unless there is a special reason.
【０００３】[0003]
【発明が解決しようとする課題】シリコン単結晶は高純
度であることが要求されている。しかし、上記シリコン
単結晶の引き上げ過程において、黒鉛るつぼから発生す
る重金属蒸気が石英るつぼ内のシリコン融液を汚染し、
成長中のシリコン単結晶の品質を低下させる。更に、黒
鉛るつぼの使用回数が重なると発生する重金属の量も増
加し、これに伴ってシリコン融液の汚染度が高くなるた
め、シリコン単結晶内に酸素誘起欠陥（ＯＳＦともい
う）が発生しやすくなる。前記酸素誘起欠陥の発生原因
として、るつぼからの酸素供給量、るつぼ回転速度、単
結晶回転速度、融液温度その他の影響とともに黒鉛るつ
ぼから発生する重金属蒸気も原因の一つと考えられる。
酸素誘起欠陥の調査は図５に示すように、シリコン単結
晶のボデイ部を４分割し、４個の試料Ｓ1 ，Ｓ2 ，Ｓ3
，Ｓ4 を酸化熱処理、エッチングの上、顕微鏡観察に
よって欠陥数を算出する。従来は、酸素誘起欠陥が許容
値を超えると黒鉛るつぼを新品と交換しているが、酸素
誘起欠陥調査に多大の工数を要し、また、酸素誘起欠陥
調査結果に基づいて黒鉛るつぼの継続使用可否を決定す
る従来の方法では、酸素誘起欠陥の発生を未然に防止す
ることができない。本発明は上記従来の問題点に着目し
てなされたもので、シリコン単結晶の引き上げ過程にお
いて、黒鉛るつぼから発生する重金属蒸気の濃度を測定
し、黒鉛るつぼの交換の要否を判定するための黒鉛るつ
ぼの使用限度判定装置および判定方法を提供することを
目的としている。The silicon single crystal is required to have high purity. However, in the process of pulling the silicon single crystal, heavy metal vapor generated from the graphite crucible contaminates the silicon melt in the quartz crucible,
Deteriorates the quality of the growing silicon single crystal. Furthermore, when the number of times of use of the graphite crucible is increased, the amount of heavy metal generated also increases, and the degree of contamination of the silicon melt increases accordingly. As a result, oxygen-induced defects (OSF) occur in the silicon single crystal. It will be easier. One of the causes of the oxygen-induced defects is considered to be the heavy metal vapor generated from the graphite crucible together with the influence of the oxygen supply amount from the crucible, the crucible rotation speed, the single crystal rotation speed, the melt temperature and the like.
As shown in FIG. 5, the body portion of the silicon single crystal was divided into four parts, and four samples S1, S2 and S3 were examined.
, S4 are subjected to oxidation heat treatment and etching, and the number of defects is calculated by microscopic observation. Conventionally, graphite crucibles are replaced with new ones when the oxygen-induced defects exceed the allowable value.However, it takes a lot of man-hours to investigate oxygen-induced defects, and the continuous use of graphite crucibles based on the results of oxygen-induced defect investigations. With the conventional method of determining whether or not it is possible, it is not possible to prevent the occurrence of oxygen-induced defects. The present invention has been made in view of the above-described conventional problems, and measures the concentration of heavy metal vapor generated from a graphite crucible in the process of pulling a silicon single crystal to determine whether the graphite crucible needs to be replaced. It is an object of the present invention to provide an apparatus and method for determining a use limit of a graphite crucible.
【０００４】[0004]
【課題を解決するための手段】上記目的を達成するた
め、本発明に係る黒鉛るつぼの使用限度判定装置は、Ｃ
Ｚ法によるシリコン単結晶製造装置に付設する判定装置
であって、黒鉛るつぼの上端から発生する重金属蒸気の
濃度を測定する手段と、前記濃度の測定値に基づいて黒
鉛るつぼの使用限度を判定する手段および使用限度であ
ることを表示する手段とからなる構成とし、このような
構成において、重金属蒸気の濃度を測定する手段が、黒
鉛るつぼの上端に近接して黒鉛るつぼの上端面を包囲す
るように設けた包囲体と、前記包囲体の内部に蓄積され
た重金属蒸気を吸引するガス導引管と、差動排気装置
と、重金属蒸気の成分・濃度を分析・測定する質量分析
計とからなるものとした。また、上記使用限度判定装置
を用いる黒鉛るつぼの使用限度判定方法は、ＣＺ法によ
るシリコン単結晶の引き上げ過程において、黒鉛るつぼ
の上端から発生し、包囲体の内部に蓄積された重金属蒸
気をガス導引管により吸引し、差動排気装置により所定
の真空度まで減圧した上、質量分析計に導いて重金属蒸
気の成分・濃度を分析・測定し、重金属蒸気の濃度が許
容値を超えたとき、これを表示する表示灯が点灯すると
ともに、次の引き上げ作業を停止させるように制御する
こととした。In order to achieve the above object, an apparatus for determining the use limit of a graphite crucible according to the present invention comprises:
A determination device attached to a silicon single crystal manufacturing apparatus based on the Z method, comprising: means for measuring a concentration of heavy metal vapor generated from an upper end of a graphite crucible; and determining a use limit of the graphite crucible based on the measured value of the concentration. Means and means for indicating that the use limit has been reached.In such a structure, the means for measuring the concentration of heavy metal vapor surrounds the upper end surface of the graphite crucible close to the upper end of the graphite crucible. And a gas guide tube for sucking heavy metal vapor accumulated inside the enclosure, a differential exhaust device, and a mass spectrometer for analyzing and measuring the component and concentration of heavy metal vapor. It was taken. Further, the method for determining the use limit of a graphite crucible using the above-mentioned use limit determination device is a method in which heavy metal vapor generated from the upper end of the graphite crucible and accumulated inside the enclosure is gas-conducted in the process of pulling the silicon single crystal by the CZ method. Suction is performed by a draw tube, and the pressure is reduced to a predetermined degree of vacuum by a differential exhaust device.Then, the component is introduced to a mass spectrometer to analyze and measure the component and concentration of the heavy metal vapor. An indicator light indicating this is turned on, and control is performed so as to stop the next lifting operation.
【０００５】[0005]
【作用】上記構成によれば、黒鉛るつぼの上端面を包囲
するように包囲体を設けたので、黒鉛るつぼの上端から
発生する重金属蒸気の大部分を前記包囲体によって捕捉
することができ、重金属によるシリコン融液の汚染を防
止することができる。包囲体内に蓄積された重金属蒸気
はガス導引管と、差動排気装置とを経て質量分析計に導
かれるので、重金属蒸気の成分・濃度を分析・測定する
ことができ、重金属蒸気の濃度が許容値を超えたとき
は、表示灯が点灯するので、黒鉛るつぼが使用限度であ
ることを容易に認識することができる。According to the above construction, since the enclosure is provided so as to surround the upper end surface of the graphite crucible, most of the heavy metal vapor generated from the upper end of the graphite crucible can be captured by the enclosure. Contamination of the silicon melt can be prevented. The heavy metal vapor accumulated in the enclosure is guided to the mass spectrometer through the gas guide tube and the differential exhaust device, so that the component and concentration of the heavy metal vapor can be analyzed and measured, and the concentration of the heavy metal vapor is reduced. When the allowable value is exceeded, the indicator light is turned on, so that it can be easily recognized that the graphite crucible is at the usage limit.
【０００６】[0006]
【実施例】以下に本発明に係る黒鉛るつぼの使用限度判
定装置および判定方法の実施例について、図面を参照し
て説明する。図１は本装置の概略構成を示し、図２はる
つぼおよびるつぼ周辺の断面説明図である。これらの図
において、シリコン融液１を貯留するるつぼは、黒鉛る
つぼ２の内側に石英るつぼ３を嵌着したもので、前記る
つぼの上方には、黒鉛るつぼ２と石英るつぼ３との接合
面および黒鉛るつぼ２の上端面を被覆する包囲体４が設
けられている。この包囲体４は、断面がほぼコの字状の
環で、開口部を下向きにし、るつぼの上端面に近接して
配設され、包囲体４の上面には複数個のガス導引管５の
一端がそれぞれ固着されている。上記において包囲体は
一部被覆する逆漏斗にガス導引管に接続しても良い。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a block diagram showing an embodiment of an apparatus and method for judging the use limit of a graphite crucible according to the present invention. FIG. 1 shows a schematic configuration of the present apparatus, and FIG. 2 is an explanatory cross-sectional view of a crucible and a periphery of the crucible. In these figures, a crucible for storing a silicon melt 1 has a quartz crucible 3 fitted inside a graphite crucible 2, and a joining surface between the graphite crucible 2 and the quartz crucible 3 is provided above the crucible. An enclosure 4 that covers the upper end surface of the graphite crucible 2 is provided. The surrounding body 4 is a ring having a substantially U-shaped cross section, the opening is directed downward, and is disposed close to the upper end surface of the crucible. Are respectively fixed at one end. In the above, the enclosure may be connected to the gas guiding tube in the reverse funnel partially covered.
【０００７】前記ガス導引管５は、内壁に金属蒸気が付
着することを防止するため、長さの短い直管が用いられ
ている。ガス導引管５の他端は差動排気装置６に接続さ
れ、差動排気装置６と質量分析計７とは管８によって接
続されている。前記質量分析計７は、気化した金属分子
をイオン化して分子量、分子の構造を測定するもので、
たとえば四重極質量分析計、磁場型質量分析計等が用い
られ、質量分析計７の出力配線は制御装置１０の直流増
幅器１１、サンプルホールド回路１２、Ａ／Ｄ変換器１
３および入出力ポート１４を介して中央処理装置（以下
ＣＰＵという）１５に接続されている。また、記憶装置
１６は前記ＣＰＵ１５に接続され、ＣＰＵ１５は質量分
析計７で得られた実測値と前記許容値とを比較する比較
部と、実測値が許容値を超えた場合に単結晶製造装置の
表示灯９を点灯する制御部とからなっている。The gas guide tube 5 is a straight tube having a short length in order to prevent metal vapor from adhering to the inner wall. The other end of the gas guide tube 5 is connected to a differential exhaust device 6, and the differential exhaust device 6 and the mass spectrometer 7 are connected by a tube 8. The mass spectrometer 7 ionizes vaporized metal molecules and measures the molecular weight and molecular structure.
For example, a quadrupole mass spectrometer, a magnetic field type mass spectrometer, or the like is used.
The CPU 3 is connected to a central processing unit (hereinafter referred to as a CPU) 15 through an input / output port 3 and an input / output port 14. Further, the storage device 16 is connected to the CPU 15, the CPU 15 compares the measured value obtained by the mass spectrometer 7 with the permissible value, and a single crystal manufacturing apparatus when the measured value exceeds the permissible value. And a control unit for turning on the indicator light 9.
【０００８】シリコン単結晶の引き上げに当たり、チャ
ンバ内を低真空度とし、好ましくは１０ｔｏｒｒ以下に
保つ。ヒータの加熱によって黒鉛るつぼ２の温度が上昇
すると、黒鉛るつぼ２に含まれている大部分の重金属は
上下方向に移動する。上方に移動した重金属蒸気は包囲
体４内に蓄積され、チャンバ内への拡散が抑制される。
包囲体４内に蓄積された重金属蒸気はガス導引管５に吸
引され、差動排気装置６によって真空度を高めた後、質
量分析計７のイオン化室７ａに導かれてイオン化され
る。更にイオン分離室７ｂ内で各重金属ごとに分離さ
れ、分離した順にイオン検出部７ｃで分析された上、電
流に変換される。変換された電流は制御装置１０の直流
増幅器１１によって増幅された後、電圧として出力さ
れ、一定時間サンプルホールド回路１２により前記出力
値を保持し、その間Ａ／Ｄ変換器１３によりアナログ値
をデジタル値に変換される。前記変換値は入出力ポート
１４を介してＣＰＵ１５に入力され、記憶装置１６に記
録される。このようにして前記の各重金属濃度は順次記
憶装置１６に記録され、この工程が一巡すると、今回の
測定値を前回の測定値に加算する。これらの操作を複数
回繰り返した後、加算した累計値がそれぞれの重金属濃
度の許容値を１個もしくは複数個について超えたとき、
黒鉛るつぼの交換時期を示す表示灯９が点灯する。この
場合は引き上げ作業終了後、次の作業は再開されない。In pulling the silicon single crystal, the inside of the chamber is kept at a low vacuum, and preferably kept at 10 torr or less. When the temperature of the graphite crucible 2 rises due to the heating of the heater, most of the heavy metals contained in the graphite crucible 2 move up and down. The heavy metal vapor that has moved upward is accumulated in the enclosure 4 and diffusion into the chamber is suppressed.
The heavy metal vapor accumulated in the enclosure 4 is sucked into the gas guide tube 5, the degree of vacuum is increased by the differential exhaust device 6, and then guided to the ionization chamber 7 a of the mass spectrometer 7 to be ionized. Furthermore, each heavy metal is separated in the ion separation chamber 7b, analyzed by the ion detection unit 7c in the order of separation, and converted into a current. The converted current is amplified by the DC amplifier 11 of the control device 10 and then output as a voltage. The output value is held by the sample and hold circuit 12 for a certain period of time, during which the analog value is converted into a digital value by the A / D converter 13. Is converted to The converted value is input to the CPU 15 via the input / output port 14 and recorded in the storage device 16. In this way, the respective heavy metal concentrations are sequentially recorded in the storage device 16, and when this process is completed, the current measured value is added to the previous measured value. After repeating these operations a plurality of times, when the sum total exceeds the allowable value of each heavy metal concentration for one or more,
The indicator light 9 indicating the time for replacing the graphite crucible is turned on. In this case, after the lifting operation is completed, the next operation is not restarted.
【０００９】重金属蒸気の分析はシリコン単結晶の引き
上げ工程の最初から終了まで連続して、もしくは定期的
に行われる。また、引き上げ工程の再開とともに前期分
析も再開される。採取された各重金属蒸気の分析値は、
各重金属濃度の許容値として設定、記憶した判定値と比
較される。１個もしくは複数の分析値が判定値を超える
と、石英るつぼ内に混入する重金属の量も許容値を超え
たものと判定され、黒鉛るつぼの交換時期がきたことを
示す表示灯９が点灯する。前記各重金属蒸気の分析値
は、るつぼ使用のつど採取した各重金属蒸気の測定値の
総和でも平均値でもよく、また、最適と考えた一時期に
採取した各重金属蒸気の測定値でもよい。The analysis of heavy metal vapor is performed continuously or periodically from the beginning to the end of the silicon single crystal pulling step. In addition, the analysis in the first half will be restarted with the restart of the lifting process. The analytical value of each collected heavy metal vapor is
Each heavy metal concentration is compared with a determination value set and stored as an allowable value. When one or more analysis values exceed the determination value, it is determined that the amount of heavy metal mixed in the quartz crucible also exceeds the allowable value, and the indicator light 9 indicating that the time for replacing the graphite crucible has come on is lit. . The analysis value of each heavy metal vapor may be the sum or average value of the measurement values of each heavy metal vapor sampled each time the crucible is used, or may be the measurement value of each heavy metal vapor sampled at one time considered to be optimal.
【００１０】図３は、黒鉛るつぼの使用回数と、本発明
による黒鉛るつぼの使用限度判定装置が測定した重金属
濃度との関係を示す図である。黒鉛るつぼの使用回数が
１０回以下の場合は、蒸発重金属の濃度が低い。しか
し、使用回数が１０回を超えると前記濃度は急上昇す
る。また、図４は黒鉛るつぼの使用回数と酸素誘起欠陥
発生数との関係を示す図である。酸素誘起欠陥発生数の
測定は図５に示すように、シリコン単結晶のボデイ部を
４分割し、４個の試料Ｓ1 ，Ｓ2 ，Ｓ3 ，Ｓ4 を酸化熱
処理、エッチング処理した上、顕微鏡観察により行っ
た。ボデイ部の酸素誘起欠陥発生数は、黒鉛るつぼの使
用回数が１０回以下では不良と見做す程の量ではない
が、１０回を超えると急激に増加する。このような現象
は、黒鉛るつぼから蒸発した重金属の一部が石英るつぼ
の中に拡散し、融液に混入して引き上げ単結晶に欠陥を
発生させるものと考えられる。FIG. 3 is a graph showing the relationship between the number of times the graphite crucible is used and the heavy metal concentration measured by the graphite crucible use limit determining apparatus according to the present invention. When the number of uses of the graphite crucible is 10 or less, the concentration of the evaporated heavy metal is low. However, when the number of times of use exceeds 10, the concentration sharply increases. FIG. 4 is a graph showing the relationship between the number of times the graphite crucible is used and the number of oxygen-induced defects. As shown in FIG. 5, the number of oxygen-induced defects was measured by dividing the body of a silicon single crystal into four parts, subjecting four samples S1, S2, S3, and S4 to an oxidizing heat treatment and an etching treatment, followed by microscopic observation. Was. The number of occurrences of oxygen-induced defects in the body portion is not so large as to be regarded as defective when the number of times of use of the graphite crucible is less than 10, but increases sharply when the number exceeds 10 times. It is considered that such a phenomenon is that a part of the heavy metal evaporated from the graphite crucible diffuses into the quartz crucible, mixes with the melt, and causes a defect in the pulled single crystal.
【００１１】図３と図４とを比較すると、互いに相関が
あることが分かる。すなわち、黒鉛るつぼの使用回数ご
とに発生する重金属蒸気が急増する時期と、シリコン単
結晶中の酸素誘起欠陥が急増する時期とがおおよそ一致
している。従って、黒鉛るつぼの使用回数ごとに測定す
る蒸発重金属濃度測定値から黒鉛るつぼの交換時期を決
定することができる。A comparison between FIG. 3 and FIG. 4 shows that there is a correlation therebetween. In other words, the time when the heavy metal vapor generated every time the graphite crucible is used suddenly increases and the time when the oxygen-induced defects in the silicon single crystal rapidly increase coincide with each other. Therefore, the replacement time of the graphite crucible can be determined from the measured value of the concentration of the evaporated heavy metal measured each time the graphite crucible is used.
【００１２】[0012]
【発明の効果】以上説明したように本発明によれば、黒
鉛るつぼの上端面を包囲するように包囲体を設け、黒鉛
るつぼの上端から発生する重金属蒸気の大部分を前記包
囲体によって捕捉することにしたので、重金属の拡散に
よるシリコン融液の汚染を防止することができる。そし
て、包囲体内に蓄積された重金属蒸気はガス導引管と、
差動排気装置とを経て質量分析計に導かれ、質量分析計
によって分析・測定された重金属蒸気の成分・濃度はＣ
ＰＵにより許容値と比較され、重金属蒸気の濃度が許容
値を超えたときは、表示灯を点灯させることにしたの
で、黒鉛るつぼが使用限度に到達したことを容易に認識
することができる。このように黒鉛るつぼの使用回数
を、黒鉛るつぼから発生する重金属濃度によって的確に
管理することにより、シリコン単結晶の品質を高純度に
維持することができるとともに、酸素誘起欠陥による不
良発生を未然に防止することが可能となる。As described above, according to the present invention, an enclosure is provided so as to surround the upper end surface of the graphite crucible, and most of the heavy metal vapor generated from the upper end of the graphite crucible is captured by the enclosure. Therefore, contamination of the silicon melt by the diffusion of the heavy metal can be prevented. And the heavy metal vapor accumulated in the enclosure inside the gas guide tube,
The component and concentration of the heavy metal vapor analyzed and measured by the mass spectrometer through the differential evacuation device are introduced into the mass spectrometer.
It is compared with the allowable value by the PU, and when the concentration of the heavy metal vapor exceeds the allowable value, the indicator lamp is turned on. Therefore, it is possible to easily recognize that the graphite crucible has reached the use limit. By properly controlling the number of times the graphite crucible is used in accordance with the concentration of heavy metals generated from the graphite crucible, it is possible to maintain the quality of the silicon single crystal with high purity and to prevent the occurrence of defects due to oxygen-induced defects. This can be prevented.
【図１】黒鉛るつぼの使用限度判定装置の概略構成を示
す説明図である。FIG. 1 is an explanatory diagram showing a schematic configuration of a use limit determining device for a graphite crucible.
【図２】るつぼおよびるつぼ周辺の断面説明図である。FIG. 2 is an explanatory cross-sectional view of a crucible and a periphery of the crucible.
【図３】黒鉛るつぼの使用回数と、重金属濃度との関係
を示す図である。FIG. 3 is a diagram showing the relationship between the number of times of using a graphite crucible and the concentration of heavy metals.
【図４】黒鉛るつぼの使用回数と酸素誘起欠陥発生数と
の関係を示す図である。FIG. 4 is a diagram showing a relationship between the number of times of using a graphite crucible and the number of occurrences of oxygen-induced defects.
【図５】酸素誘起欠陥数測定試料を採取する際の、シリ
コンインゴット切断状況を示す説明図である。FIG. 5 is an explanatory diagram showing a silicon ingot cutting state when a sample for measuring the number of oxygen-induced defects is taken.
２ 黒鉛るつぼ ３ 石英るつぼ ４ 包囲体 ５ ガス導引管 ６ 差動排気装置 ７ 質量分析計 ９ 表示灯 １０ 制御装置 １５ 中央処理装置（ＣＰＵ） 2 Graphite crucible 3 Quartz crucible 4 Enclosure 5 Gas guide tube 6 Differential exhaust device 7 Mass spectrometer 9 Indicator 10 Control device 15 Central processing unit (CPU)
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) C30B 15/10 - 15/12 G01N 27/62──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. 6 , DB name) C30B 15/10-15/12 G01N 27/62
Claims (3)
付設する判定装置であって、黒鉛るつぼの上端から発生
する重金属蒸気の濃度を測定する手段と、前記濃度の測
定値に基づいて黒鉛るつぼの使用限度を判定する手段お
よび使用限度であることを表示する手段とからなること
を特徴とする黒鉛るつぼの使用限度判定装置。1. A judging device attached to a silicon single crystal manufacturing apparatus by a CZ method, comprising: means for measuring the concentration of heavy metal vapor generated from the upper end of a graphite crucible; An apparatus for determining a use limit of a graphite crucible, comprising: means for determining a use limit; and means for indicating that the use limit has been reached.
測定する手段が、黒鉛るつぼの上端に近接して黒鉛るつ
ぼの上端面を包囲するように設けた包囲体と、前記包囲
体の内部に蓄積された重金属蒸気を吸引するガス導引管
と、差動排気装置と、重金属蒸気の成分・濃度を分析・
測定する質量分析計とからなることを特徴とする黒鉛る
つぼの使用限度判定装置。2. The enclosure according to claim 1, wherein the means for measuring the concentration of the heavy metal vapor is provided so as to surround an upper end surface of the graphite crucible close to an upper end of the graphite crucible, and the inside of the enclosure. Analysis of gas components and concentrations of heavy metal vapor, gas guide tube for sucking heavy metal vapor accumulated in
A use limit determining device for a graphite crucible, comprising a mass spectrometer for measuring.
過程において、黒鉛るつぼの上端から発生し、包囲体の
内部に蓄積された重金属蒸気をガス導引管により吸引
し、差動排気装置により所定の真空度まで減圧した上、
質量分析計に導いて重金属蒸気の成分・濃度を分析・測
定し、重金属蒸気の濃度が許容値を超えたとき、これを
表示する表示灯が点灯するとともに、次の引き上げ作業
を停止させるように制御することを特徴とする黒鉛るつ
ぼの使用限度判定方法。3. In the process of pulling a silicon single crystal by the CZ method, heavy metal vapor generated from the upper end of a graphite crucible and accumulated inside the enclosure is sucked by a gas guide tube, and is subjected to a predetermined evacuation by a differential exhaust device. After reducing the pressure to a vacuum,
Introduce to the mass spectrometer to analyze and measure the component and concentration of heavy metal vapor.When the concentration of heavy metal vapor exceeds the allowable value, the indicator light will be turned on and the next lifting operation will be stopped. A method for determining a use limit of a graphite crucible, characterized by controlling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15140592A JP2814036B2 (en) | 1992-05-19 | 1992-05-19 | Apparatus and method for determining use limit of graphite crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15140592A JP2814036B2 (en) | 1992-05-19 | 1992-05-19 | Apparatus and method for determining use limit of graphite crucible |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05319977A JPH05319977A (en) | 1993-12-03 |
| JP2814036B2 true JP2814036B2 (en) | 1998-10-22 |
Family
ID=15517876
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15140592A Expired - Lifetime JP2814036B2 (en) | 1992-05-19 | 1992-05-19 | Apparatus and method for determining use limit of graphite crucible |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2814036B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020124792A1 (en) * | 2001-01-09 | 2002-09-12 | Hariprasad Sreedharamurthy | Crystal puller and method for growing single crystal semiconductor material |
| JP6881122B2 (en) * | 2017-07-20 | 2021-06-02 | 株式会社Sumco | Method for manufacturing silicon single crystal |
-
1992
- 1992-05-19 JP JP15140592A patent/JP2814036B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05319977A (en) | 1993-12-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH06132224A (en) | Semiconductor device manufacturing apparatus, load lock chamber, and semiconductor device manufacturing method using the semiconductor device manufacturing apparatus | |
| US6630363B2 (en) | Method for evaluating impurity concentrations in unpolished wafers grown by the Czochralski method | |
| JP2814036B2 (en) | Apparatus and method for determining use limit of graphite crucible | |
| WO2002057519A9 (en) | Process for monitoring the gaseous environment of a crystal puller for semiconductor growth | |
| US6216526B1 (en) | Gas sampler for molten metal and method | |
| JPH10223713A (en) | Heat treatment evaluation wafer and heat treatment evaluation method using the same | |
| JP3663774B2 (en) | Method and apparatus for analyzing trace oxygen in metal | |
| US5172183A (en) | Glow discharge atomic emission spectroscopy and apparatus thereof | |
| Clegg et al. | Determination of oxygen in semiconductor materials with a cryogenically pumped spark-source mass spectrometer | |
| JP2000009694A (en) | Quantitative analysis method and quantitative analyzer | |
| JP2000002699A (en) | Analyzer for element in sample | |
| JPH10282086A (en) | Molten metal sampling method and molten metal sampling probe | |
| WO2023159789A1 (en) | Gc-aed related technology and method for analysis and detection for ppb content of germane impurities in high purity phosphine | |
| JPH07297246A (en) | Method for monitoring metal contamination of silicon semiconductor | |
| JPH11316220A (en) | Method and apparatus for high-precision analysis of trace elements in metals | |
| EP1666877A1 (en) | Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device | |
| JP4022347B2 (en) | Analytical oxygen analysis method | |
| JPH05221782A (en) | Single crystal producing device and its control method | |
| JP2847228B2 (en) | Evaluation method of semiconductor jig material | |
| JPH0666695A (en) | Preparation of sample | |
| US7109039B1 (en) | Chemical composition for dissolving a sample taken from semiconductor device fabrication equipment and method for analyzing contaminants on the equipment using the chemical composition | |
| JP2020106369A (en) | Gas analysis method | |
| CN115541519B (en) | A method for determining the carbon blank value in a flux | |
| JPH0567665A (en) | Leak detection method | |
| CN119880561A (en) | Pretreatment method and detection method for detecting vanadium-zirconium-iron alloy sample by glow discharge mass spectrum |