TWI727410B - Method for producing single crystal silicon ingot and apparatus for pulling silicon single crystal - Google Patents
Method for producing single crystal silicon ingot and apparatus for pulling silicon single crystal Download PDFInfo
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
Description
本發明,係有關於單結晶矽鑄錠的製造方法及矽單結晶拉引裝置。The present invention relates to a manufacturing method of a single crystal silicon ingot and a silicon single crystal pulling device.
作為半導體元件的基板使用的矽晶圓,係透過薄切矽單結晶的鑄錠,經由平面研磨(lapping)步驟、蝕刻步驟以及鏡面研磨(polishing),最後洗淨製造。於是。300mm以上的大口徑矽單結晶,一般以柴氏拉晶 (Czochralski, CZ) 法製造。The silicon wafer used as the substrate of the semiconductor element is manufactured through a thin-cut silicon single crystal ingot, through a lapping step, an etching step, and a mirror polishing step, and finally it is cleaned and manufactured. then. Large-diameter silicon single crystals over 300mm are generally manufactured by the Czochralski (CZ) method.
第4圖,顯示利用CZ 法製造單結晶矽鑄錠的習知矽單結晶拉引裝置400。矽單結晶拉引裝置400,其外圍以密室10構成,其中心部配置坩堝16。坩堝16具有兩層構造,由內側的石英坩堝16A與外側的黑鉛坩堝16B構成,以軸驅動機構20固定至可旋轉及升降的傳動軸18上端部。Figure 4 shows a conventional silicon single
坩堝16的外側,圍繞坩堝16配設電阻加熱式的筒狀加熱器24,其外側沿著密室10的內側面配設斷熱體26。又,坩堝16的上方,與傳動軸18同軸上配置在下端保持保持種晶S 的種晶夾頭28之拉引線30,以既定的速度往與傳動軸18反方向或相同方向旋轉的同時,升降線升降機構32。On the outside of the
密室10內,在坩堝16上方圍繞生長中的單結晶矽鑄錠I配置筒狀的熱遮蔽體22。此熱遮蔽體22,調整對於生長中的鑄錠I之來自坩堝16內矽融液M、加熱器24和坩堝16側壁的高溫輻射熱入射量,擔任控制單結晶矽鑄錠I的中心部及外周部往拉引軸X方向的溫度斜度的任務。
In the closed
密室10的上部,設置導入Ar(氬)氣體等非活性氣體至密室10內的氣體導入口12。又,密室10的底部,設置利用未圖示的真空泵的驅動吸引排出密室10內的氣體之氣體排出口14。從氣體導入口12導入密室10內的非活性氣體,從生長中的單結晶矽鑄錠I與熱遮蔽體22之間下降,流過熱遮蔽體22的下端與矽融液M液面的間隙後,往熱遮蔽體22的外側,更往坩堝16的外側流動,之後從坩堝16的外側下降,從氣體排出口14排出。
The upper part of the closed
使用此矽單結晶拉引裝置400,維持密室10內在減壓下的Ar氣體空氣中的狀態下,利用加熱器24的加熱溶融坩堝16內填充的多晶矽等矽原料,形成矽融液M。其次,利用線升降機構32降下拉引線30,使種晶S接觸矽融液M,往既定方向旋轉坩堝16及拉引線30,往上方提拉拉引線30,往種晶S的下方生長鑄錠I。又,隨著鑄錠I的生長,雖然矽融液M的量減少,但上升坩堝16,維持融液面的水平。
Using this silicon single
密室10上部的開口部34中設置CCD攝影機36。CCD攝影機36,拍攝單結晶矽鑄錠I與融液M的邊界部近旁。在結晶與融液的邊界部形成的彎月面(meniscus),因為藉由比結晶及融液更高亮度拍攝,影像中的彎月面,顯現環狀高亮度帶(以下,稱作「熔環(fusion ring)」)。辨識此熔環(fusion ring)的間隔為結晶直徑,控制結晶拉引速度與融液溫度,使此結晶直徑成為所希望的一定值。
A
使用如此的矽單結晶拉引裝置的單結晶矽鑄錠的製造中,密室內產生CO氣體是眾所周知的。其原因之一,例如由於矽融液產生的SiO氣體與密室內存在的黑鉛材(例如,筒狀加熱器)的反應,產生CO氣體。專利文獻1有測量此密室內CO氣體濃度的技術。
In the manufacture of a single crystal silicon ingot using such a silicon single crystal pulling device, it is well known that CO gas is generated in a closed chamber. One of the reasons for this is, for example, the reaction of SiO gas generated from the silicon melt with the black lead material (for example, a cylindrical heater) present in the closed chamber to generate CO gas.
專利文獻1中,記載「以柴氏拉晶(Czochralski,CZ)法從加熱溶融原料的原料融液提拉單結晶之單結晶的製造方法,其特徵在於:收納上述原料在石英坩堝內,一邊加熱溶融上述石英坩堝內收納的原料,一邊測量往原料溶融中排出的排氣內包含的一氧化碳濃度,根據測量的原料溶融中排氣內包含的一氧化碳濃度測量結果,判定原料的溶融結束,之後,從上述原料融液提拉單結晶 (申請專利範圍第6項)」。
[先行技術文獻]
[專利文獻]
[專利文獻1]日本專利第2017-114709公開公報[Patent Document 1] Japanese Patent Publication No. 2017-114709
[發明所欲解決的課題][The problem to be solved by the invention]
本發明者們,著眼於在利用習知的矽單結晶拉引裝置製造的單結晶矽鑄錠中,其生長過程中混入碳,結果,以上述鑄錠製作的矽晶圓的碳濃度意外變高的課題。矽晶圓中的碳濃度變高時,元件熱處理步驟中,產生稱作殺傷缺陷的電活性碳起因的缺陷,產生降低晶圓生命期的問題。又,因為高濃度的碳促進氧析出物的形成,假設氧析出物存在元件表面上時,產生漏泄不良(leak failure),成為成品率低下的原因。這樣,對單結晶矽鑄錠中的碳污染,在半導體元件的製作步驟中產生不好的影響。因此,單結晶矽鑄錠中的碳濃度根據元件的種類以規格嚴格限制。The inventors of the present invention focused on the single crystal silicon ingot manufactured by the conventional silicon single crystal pulling device, in which carbon was mixed during the growth process. As a result, the carbon concentration of the silicon wafer produced by the above ingot unexpectedly changed. High subject. When the carbon concentration in the silicon wafer becomes higher, defects caused by electroactive carbon called killing defects are generated in the heat treatment step of the device, which causes the problem of reducing the life cycle of the wafer. In addition, because the high concentration of carbon promotes the formation of oxygen precipitates, if the oxygen precipitates are present on the surface of the device, leak failure occurs, which is a cause of low yield. In this way, the carbon contamination in the single crystal silicon ingot has a bad influence on the manufacturing steps of the semiconductor element. Therefore, the carbon concentration in the single crystal silicon ingot is strictly limited by the specifications according to the type of the device.
結晶中的碳濃度上升的理由,認為是矽融液內取入密室內產生的CO氣體。專利文獻1中,著眼於原料溶融步驟中原料全部溶融時密室內的氣體中CO氣體濃度變最大,測量CO氣體濃度,根據此測量值判定原料溶融步驟的結束(溶融結束)。但是,專利文獻1中,過於著眼於根據溶融結束的正確偵測縮短處理時間與防止石英坩堝變形,關於矽融液內取入CO氣體或起因於此的結晶中的碳濃度上升,毫無著眼。The reason for the increase in the carbon concentration in the crystal is believed to be the CO gas generated in the closed chamber taken into the silicon melt. In
有鑑於上述課題,本發明的目的在於提供可以高成品率製造碳濃度低的單結晶矽鑄錠的單結晶矽鑄錠的製造方法及矽單結晶拉引裝置。 [用以解決課題的手段]In view of the above-mentioned problems, an object of the present invention is to provide a single crystal silicon ingot manufacturing method and a silicon single crystal pulling device that can manufacture a single crystal silicon ingot with a low carbon concentration in a high yield. [Means to solve the problem]
應解決上述課題的本發明者們,構思代替監視密室內氣體中的CO氣體濃度,監視CO氣體產生率(每單位時間的CO氣體產生量)。即,認為矽融液內CO氣體的取入量與每單位時間的CO氣體產生量有正相關。另一方面,CO氣體濃度,即使每單位時間的CO氣體產生量相同,也在密室內非活性氣體的流量大時變小,且在密室內非活性氣體的流量小時變大。實際上,原料溶融步驟與結晶生長步驟中非活性氣體的流量不同,且結晶生長步驟中非活性氣體的流量變動。因此,CO氣體濃度,不適於作為評估矽融液內CO氣體的取入量的指標進行監視。本發明者們,發現藉由測量密室內的CO氣體濃度,將此測量值乘以密室內的內非活性氣體流量,算出CO氣體產生率,監視此CO氣體產生率,可以適當評估不僅矽融液內CO氣體的取入量甚至結晶中的碳濃度。The inventors of the present invention who should solve the above-mentioned problems have conceived of monitoring the CO gas generation rate (CO gas generation amount per unit time) instead of monitoring the CO gas concentration in the air in the secret chamber. That is, it is considered that the amount of CO gas taken in the silicon melt is positively correlated with the amount of CO gas generated per unit time. On the other hand, the CO gas concentration, even if the CO gas production amount per unit time is the same, becomes smaller when the flow rate of the inert gas in the secret chamber is large, and becomes larger when the flow rate of the inert gas in the secret chamber is small. In fact, the flow rate of the inert gas in the raw material melting step and the crystal growth step are different, and the flow rate of the inert gas in the crystal growth step fluctuates. Therefore, the CO gas concentration is not suitable for monitoring as an indicator for evaluating the amount of CO gas taken in the silicon melt. The inventors found that by measuring the CO gas concentration in the secret chamber, multiplying the measured value by the internal inert gas flow rate in the secret chamber, calculating the CO gas generation rate, and monitoring the CO gas generation rate, it is possible to properly evaluate not only the silicon melt The amount of CO gas taken in the liquid or even the carbon concentration in the crystal.
本發明,根據上述的見解完成,其主旨構成如下。 (1) 單結晶矽鑄錠的製造方法,使用矽單結晶拉引裝置進行,上述矽單結晶拉引裝置包括: 密室,上部具有導入非活性氣體的氣體導入口,底部具有排出包含上述非活性氣體的爐內氣體之氣體排出口; 坩堝,位於上述密室內;以及 筒狀加熱器,位於上述密室內圍繞上述坩堝; 上述製造方法,包括: 原料溶融步驟,減壓下一邊維持上述密室內在上述非活性氣體空氣中,一邊利用上述加熱器加熱、溶融投入上述坩堝內的矽原料,在上述坩堝內形成矽融液;以及 結晶生長步驟,接著,減壓下一邊維持上述密室內在上述非活性氣體空氣中,一邊利用上述加熱器加熱、維持上述矽融液,再從上述矽融液提拉單結晶矽鑄錠; 其中,上述原料溶融步驟以及上述結晶生長步驟中, 採集上述爐內氣體; 間歇以氣體分析裝置測量上述採集的氣體中的CO(一氧化碳) 氣體濃度; 測量的CO氣體濃度,乘以供給至上述密室內的非活性氣體流量,藉此算出CO氣體產生率; 監視算出的上述CO氣體產生率。The present invention has been completed based on the above findings, and its gist is structured as follows. (1) The manufacturing method of a single crystal silicon ingot is carried out by using a silicon single crystal pulling device. The above silicon single crystal pulling device includes: Closed chamber, the upper part has a gas inlet for introducing inert gas, and the bottom has a gas outlet for discharging the gas in the furnace containing the above-mentioned inert gas; The crucible is located in the aforementioned chamber; and A cylindrical heater located in the above-mentioned closed chamber and surrounding the above-mentioned crucible; The above manufacturing method includes: In the raw material melting step, while maintaining the enclosed chamber in the inert gas air under reduced pressure, the heater is used to heat and melt the silicon raw material put into the crucible to form a silicon melt in the crucible; and The crystal growth step, then, while maintaining the enclosed chamber in the inert gas air under reduced pressure, heating and maintaining the silicon melt with the heater, and then pulling the single crystal silicon ingot from the silicon melt; Wherein, in the above-mentioned raw material melting step and the above-mentioned crystal growth step, Collect the above-mentioned furnace gas; Intermittently measure the CO (carbon monoxide) gas concentration in the collected gas with a gas analysis device; The measured CO gas concentration is multiplied by the inert gas flow rate supplied to the aforementioned chamber to calculate the CO gas generation rate; Monitor the calculated CO gas generation rate.
(2) 上述(1)中記載的單結晶矽鑄錠的製造方法,其中,上述原料溶融步驟中CO氣體產生率的最大值為A(mol/h(莫耳/小時)),上述結晶生長步驟中的直幹步驟中CO氣體產生率的最大值為B(mol/h),上述原料溶融步驟以及上述結晶生長步驟,在滿足A/B≦10的條件下進行。(2) The method for producing a single crystal silicon ingot as described in (1) above, wherein the maximum value of the CO gas generation rate in the raw material melting step is A (mol/h (mol/h)), and the crystal grows The maximum value of the CO gas generation rate in the direct drying step in the steps is B (mol/h), and the above-mentioned raw material melting step and the above-mentioned crystal growth step are performed under the condition that A/B≦10.
(3) 上述(1)或(2)中記載的單結晶矽鑄錠的製造方法,其中,上述爐內氣體的採集,經由從上述氣體排出口延伸的排氣配管進行。(3) The method for producing a single crystal silicon ingot as described in (1) or (2), wherein the gas in the furnace is collected via an exhaust pipe extending from the gas discharge port.
(4) 上述(1)至(3)中任一項記載的單結晶矽鑄錠的製造方法,其中,上述爐內氣體,從設置在上述坩堝上方圍繞上述單結晶矽鑄錠的筒狀熱遮蔽體以及上述坩堝之間的空間採集。(4) The method for producing a single crystal silicon ingot according to any one of (1) to (3), wherein the gas in the furnace is heated from a cylindrical heat set above the crucible and surrounding the single crystal silicon ingot The space between the shielding body and the crucible is collected.
(5) 上述(1)至(4)中任一項記載的單結晶矽鑄錠的製造方法,其中,上述氣體分析裝置是四層極型質量分析裝置。(5) The method for producing a single crystal silicon ingot according to any one of (1) to (4) above, wherein the gas analyzer is a four-layer pole type mass analyzer.
(6) 矽單結晶拉引裝置,其特徵在於包括: 密室,上部具有導入非活性氣體的氣體導入口,底部具有排出包含上述非活性氣體的爐內氣體之氣體排出口; 坩堝,位於上述密室內,收納矽融液;以及 筒狀熱遮蔽體,設置在上述坩堝上方,圍繞從上述矽融液提拉的單結晶矽鑄錠; 筒狀加熱器,位於上述密室內圍繞上述坩堝,加熱上述矽融液; 排氣配管,從上述氣體排出口延伸; 主泵,連接至上述排氣配管,減壓上述密室內的同時,吸引上述爐內氣體往上述排氣配管; 主閥,設置在上述排氣配管,減壓上述密室內之際為打開; 採集口,設置在上述排氣配管的上述主閥的上游部位以及上述熱遮蔽體與上述坩堝之間的空間其中一方或兩方; 次配管,從上述氣體採集口延伸,連結至上述排氣配管的上述主閥的下游部位; 次泵,設置在上述次配管中,吸引上述爐內氣體往上述次配管; 氣體分析裝置,設置在上述次配管的上述次泵的上游,間歇測量吸引至上述次配管的氣體中的CO氣體濃度; 流量調整閥,設置在上述次配管的上述氣體分析裝置的上游,調整供給至上述氣體分析裝置的氣體流量; 過濾器,設置在上述次配管的上述流量調整閥的上游,除去吸引至上述次配管的氣體中的SiO粉;以及 取入閥,設置在上述次配管的上述氣體採集口近旁,吸引上述爐內氣體往上述次配管之際為打開; 更包括: 演算部,將根據上述氣體分析裝置測量的CO氣體濃度,乘以供給上述密室內的非活性氣體流量,藉此算出CO氣體產生率;以及 輸出裝置,輸出算出的上述CO氣體產生率。(6) Silicon single crystal pulling device, characterized by including: Closed chamber, the upper part has a gas inlet for introducing inert gas, and the bottom has a gas outlet for discharging the gas in the furnace containing the above-mentioned inert gas; The crucible is located in the above-mentioned closed chamber and contains the silicon melt; and A cylindrical heat shield is set above the crucible and surrounds the single crystal silicon ingot pulled from the silicon melt; A cylindrical heater, located in the above-mentioned closed chamber, surrounding the above-mentioned crucible, and heating the above-mentioned silicon melt; Exhaust piping extending from the above-mentioned gas discharge port; The main pump is connected to the exhaust piping, and while depressurizing the secret chamber, it sucks the gas in the furnace to the exhaust piping; The main valve is set in the exhaust pipe, and opens when the pressure is reduced in the closed chamber; The collection port is provided at one or both of the upstream portion of the main valve of the exhaust piping and the space between the heat shield and the crucible; The secondary piping extends from the gas collection port and is connected to the downstream portion of the main valve of the exhaust piping; The secondary pump is installed in the secondary piping to suck the gas in the furnace to the secondary piping; A gas analysis device is installed upstream of the secondary pump of the secondary piping, and intermittently measures the CO gas concentration in the gas sucked into the secondary piping; A flow adjustment valve, which is arranged upstream of the gas analysis device of the secondary piping, and adjusts the gas flow rate supplied to the gas analysis device; A filter is installed upstream of the flow control valve of the secondary piping, and removes SiO powder in the gas sucked into the secondary piping; and The intake valve is set near the gas collection port of the secondary piping, and opens when the gas in the furnace is sucked into the secondary piping; It also includes: An arithmetic unit, multiplying the CO gas concentration measured by the gas analysis device by the inert gas flow rate supplied to the secret chamber, thereby calculating the CO gas generation rate; and The output device outputs the calculated CO gas generation rate.
(7) 上述(6)中記載的矽單結晶拉引裝置,其中,上述氣體採集口,設置在上述排氣配管的上述主閥的上游部位。(7) The silicon single crystal pulling device described in (6) above, wherein the gas collection port is provided at an upstream portion of the main valve of the exhaust pipe.
(8) 上述(6)或(7)中記載的矽單結晶拉引裝置,其中,上述氣體採集口,位於上述熱遮蔽體與上述坩堝之間的空間。(8) The silicon single crystal pulling device described in (6) or (7), wherein the gas collection port is located in a space between the heat shield and the crucible.
(9) 上述(6)〜(8)中任一項記載的矽單結晶拉引裝置,其中,上述氣體分析裝置是四層極型質量分析裝置。 [發明效果](9) The silicon single crystal pulling device described in any one of (6) to (8) above, wherein the gas analysis device is a quadrupole type mass analysis device. [Effects of the invention]
根據本發明的單結晶矽鑄錠的製造方法及矽單結晶拉引裝置,可以高成品率製造碳濃度低的單結晶矽鑄錠。According to the method for manufacturing a single crystal silicon ingot and the silicon single crystal pulling device of the present invention, a single crystal silicon ingot with a low carbon concentration can be manufactured at a high yield.
(矽單結晶拉引裝置) (Si single crystal pulling device)
參照第1~3圖,說明關於本發明實施形態的矽單結晶拉引裝置100、200、300中共同的基本構成。又,關於這些共同的基本構成,在第~3圖中附上相同的符號。
With reference to Figs. 1 to 3, the basic structure common to the silicon single
矽單結晶拉引裝置100、200、300,具有密室10、坩堝16、傳動軸18、軸驅動機構20、筒狀熱遮蔽體22、加熱器24、筒狀斷熱體26、種晶夾頭28、拉引線30、線升降機構32、CCD攝影機36、排氣配管40以及主泵42。
The silicon single
密室10的上部,設置導入Ar氣體等非活性氣體至密室10之氣體導入口12。又,密室10的底部,設置利用主泵42(真空泵)的驅動吸引排出密室10內的氣體(以下,稱作「爐內氣體」)之氣體排出口14。
The upper part of the
坩堝16,配置在密室10的中心部,收納矽融液M。坩堝16,具有石英坩堝16A與黑鉛坩堝16B的兩層構造。石英坩堝16A,在內面直接支撐矽融液M。黑鉛坩堝16B,在石英坩堝16A的外側支撐石英坩堝16A。如第1~3圖所示,石英坩堝16A的上端比黑鉛坩堝16B的上端高,即石英坩堝16A的上端從黑鉛坩堝16B的上端突出。
The
傳動軸18,往鉛直方向貫通密室10的底部,在上端支撐坩堝16。於是,軸驅動機構20,經由傳動軸18旋轉坩堝16的同時升降坩堝16。
The
熱遮蔽體22,在坩堝16的上方,設置為圍繞從矽融液M提拉的單結晶矽鑄錠I。具體而言,熱遮蔽體22,具有倒截圓錐形的遮蔽本體22A、從此遮蔽本體22A的下端部向拉引軸X側(內側)往水平方向延伸的內側凸緣部22B以及從遮蔽本體22A的上端部向密室側(外側)往水平方向延伸的外側凸緣部22C,外側凸緣部22C固定至斷熱體26。熱遮蔽體22的機能與先前技術欄中說明的相同。
The
筒狀加熱器24,位於密室10內圍繞坩堝16。加熱器24,係以碳為素材的電阻加熱式加熱器,溶融投入坩堝16內的矽原料形成矽融液M,還進行加熱用以維持形成的矽融液M。
The
筒狀斷熱體26,在熱遮蔽體22的上端下方,沿著密室10的內側面設置。本實施形態中,更在密室內的底部配置斷熱體。不特別限定構成這些斷熱體的斷熱材,但可以舉出例如碳、氧化鋁(alumina)以及氧化鋯(zirconia)。斷熱體26,特別對密室10內熱遮蔽體22下方的區域給予保熱效果,具有容易維持坩堝16內的矽融液M之機能。斷熱體26的厚度,不特別限定,可以形成與習知相等的一般厚度,生長直徑300mm(毫米)的結晶的拉引裝置中可以形成30~90mm左右,生長直徑450mm的結晶的拉引裝置中可以形成45~100mm左右。
The
坩堝16的上方,在下端保持保持種晶S的種晶夾頭28之拉引線30配置與傳動軸18在同軸上,線升降機構32,以既定的速度往傳動軸18的反方向或相同方向旋轉拉引線30的同時升降拉引線30。
Above the
密室10上部的開口部34中設置CCD攝影機36。CCD攝影機36,拍攝單結晶矽鑄錠I與矽融液M的邊界部近旁。以得到的影像中的熔環(fusion ring)的間隔作為結晶直徑,控制結晶拉引速度與融液溫度,使此結晶直徑成為所希望的一定值。
A
排氣配管40,從氣體排出口14延伸,主泵42例如可以形成乾式泵等真空泵,連接至排氣配管40,減壓密室10內至5~100Torr(托)左右的同時,達成吸引爐內氣體至排氣配管40的作用。主閥44設置在排氣配管40中,達到轉換密室10內的壓力為常壓及減壓的作用。即,將密室10內大氣開放之際、設置.交換密室10內的構造物之際等,密室10內成為常壓時,主閥44為關閉。另一方面,包含原料溶融步驟及結晶生長步驟的密室10內成為減壓時,主閥44為打開。
The
在此,原料溶融步驟及結晶生長步驟中,密室10內產生CO氣體。其第1原因,同下。即,由於矽融液M與石英坩堝16A內面反應,從坩堝16內的矽融液M,產生SiO氣體。SiO氣體,隨著非活性氣體的流動到達加熱器24,如以下的反應式所示,由於與加熱器素材的碳反應產生CO氣體。
又,作為副生長物生長的SiC在加熱器24的表面上析出。Here, in the raw material melting step and the crystal growth step, CO gas is generated in the
第2原因,如下。即,透過互相接觸的石英坩堝16A與黑鉛坩堝16B反應,產生CO氣體。
又,作為副生長物生長的SiC,在石英坩堝16A的外周面與黑鉛坩堝16B的內周面之間析出。The second reason is as follows. That is, the
本發明的各實施形態,如上述關於密室10內產生的CO氣體,監視其每單位時間的產生量(即,CO氣體產生率)。以下,說明用於此的裝置構成。In each embodiment of the present invention, as described above, regarding the CO gas generated in the
[第1實施形態]
參照第1圖,本實施形態中,具有次配管52,從排氣配管40的主閥44的上游部位分叉,連結至主閥44的下游部位。即,氣體採集口46設置在排氣配管40的主閥44的上游部位。次配管52中,從其上游依序安裝取入閥54、過濾器58、流量調整閥60、氣體分析裝置62以及次泵64。又,本說明書中,所謂排氣配管40及次配管52的「上游」及「下游」,係關於通過各配管內的氣體流。[First Embodiment]
Referring to FIG. 1, in this embodiment, there is a
次泵64,設置在次配管52中,吸引爐內氣體(嚴格說來,吸引至排氣配管的氣體)經由氣體採集口46至次配管52。次泵64,例如可以利用組合旋轉泵與輪機分子泵的真空泵裝置構成。如既述,密室10內係5〜100Torr(托) 左右的減壓空氣,為了從此減壓空氣吸引氣體至次配管52,次配管52內必須製造更低減壓空氣。根據此觀點,由於次泵64的驅動,理想是使次配管52內的壓力(過濾器58的上游之處)在1 Torr(托)以下。The
氣體分析裝置62,設置在次配管52的次泵64的上游,間歇測量吸引至次配管的氣體中的CO氣體濃度。作為氣體分析裝置62,可以舉出四層極型質量分析裝置以及氣相層析(gas chromatography)裝置。如果是四層極型質量分析裝置,CO氣體濃度的測量間隔1秒左右的話很短。另一方面,如果是現在市售的氣相層析(gas chromatography)裝置,CO氣體濃度的測量間隔最短也是15分鐘左右。因此,本實施形態,理想是使用四層極型質量分析裝置。The
流量調整閥60,設置在次配管52的氣體分析裝置62的上游,利用開閉度的調整,達成調整供給氣體分析裝置62的氣體流量之作用。藉此,可以供給適當流量的爐內氣體至氣體分析裝置62。對氣體分析裝置62供給的氣體流量理想是4×10-1
〜4×10-4
Pa.L/分。The flow
過濾器58,設置在次配管52的流量調整閥60的上游,達到除去吸引至次配管52的氣體中SiO粉的作用。上述氣體中,冷卻從矽融液M產生的SiO氣體,包含固化形成的SiO粉。第6圖中,顯示從一般密室內採集的氣體中的SiO粉末顆粒大小分布圖表。如第6圖所示,SiO粉的一般平均粒徑是13μm左右,一般的最小粒徑是1μm。因此,本實施形態中,理想是使用可以除去粒徑1μm以上的粒子99質量%以上之具有奈米級網目尺寸的氣體過濾器。作為這樣的氣體過濾器,可以舉出日本Entegris股份有限公司製晶圓卡IISF in-line gas filter(同軸氣體過濾器) 、日本精線股份有限公司 NAS Clean Process gas line用小流量過濾器等。透過設置過濾器58在流量調整閥60的上流,迴避起因於SiO粉的流量調整閥60的開閉不良,還有迴避SiO粉混入氣體分析裝置62內。The
取入閥54,設置在次配管52的氣體採集口46近旁,吸引爐內氣體至次配管52之際為開。本實施形態中,因為原料溶融步驟以及結晶生長步驟中常進行CO氣體濃度的測量及CO氣體產生率的監視,取入閥54常打開。因此,吸引至排氣配管的氣體,其一部分取入至次配管52。The
演算部66,透過將根據氣體分析裝置62測量的CO氣體濃度乘以供給至密室10內的非活性氣體流量,算出CO氣體產生率。演算部66,可以由一般的中央演算處理裝置(CPU)或微處理單元(MPU)構成。又,作為供給至密室10內的非活性氣體流量,只要使用氣體流量設定值即可。
The
輸出裝置68,輸出演算部66算出的CO氣體產生率。輸出裝置68,可以由一般的顯示器、投影機、印表機、揚聲器等構成。
The
本實施形態中,根據上述構成,代替爐內氣體的CO氣體濃度,可以即時監視爐內氣體的CO氣體產生率。這樣,藉由現場(in-situ)監視CO氣體產生率,可以適當評估不僅矽融液內CO氣體的取入量甚至結晶中的碳濃度。 In this embodiment, according to the above configuration, instead of the CO gas concentration of the furnace gas, the CO gas generation rate of the furnace gas can be monitored in real time. In this way, by monitoring the CO gas generation rate in-situ, it is possible to appropriately evaluate not only the amount of CO gas taken in the silicon melt but also the carbon concentration in the crystal.
參照第2圖,本實施形態中,氣體採集口48位於熱遮蔽體22與坩堝16之間的空間。即,從密室10的上部垂下取樣管50,使其前端的氣體採集口48位於熱遮蔽體22與坩堝16之間的空間。取樣管50,在密室10的外部與次配管52連結。取入閥56,設置在次配管52的上流側前端近旁。
Referring to FIG. 2, in this embodiment, the
第1實施形態中,對於經由次配管52採集爐內氣體,本實施形態從熱遮蔽體22與坩堝16之間的空間採集爐內氣體。關於次配管52中設置的過濾器58、流量調整閥60、氣體分析裝置62及次泵64,以及演算部66及輸出裝置68,因為與第1實施形態相同,省略說明。
In the first embodiment, with regard to collecting the gas in the furnace through the
本實施形態中,從石英坩堝的上緣直接採集爐內氣體。因此,可以直接採集與石英坩堝及黑鉛坩堝的反應產生的CO氣體。其結果,可以更高精度監視CO氣體產生率。 In this embodiment, the furnace gas is directly collected from the upper edge of the quartz crucible. Therefore, it is possible to directly collect CO gas generated by the reaction with the quartz crucible and the black lead crucible. As a result, the CO gas generation rate can be monitored with higher accuracy.
參照第3圖,本實施形態,組合第1實施形態的構成與第2實施形態的構成。即,爐內氣體的採集,經由次配管52進行,而且也從熱遮蔽體22與坩堝16之間的空間進行。Referring to Fig. 3, this embodiment combines the configuration of the first embodiment and the configuration of the second embodiment. That is, the gas in the furnace is collected via the
本實施形態中,次配管52,由第1次配管52B、第2次配管52C及第3次配管52D構成。第1次配管52B,從排氣配管40的主閥44的上游部位分叉。第2次配管52C,與取樣管50的上端連結,從密室的上部延伸。第3次配管52D,係第1次配管52B與第2次配管52C合流形成。關於取樣管50以及取入閥,與第2實施形態相同。次配管52C中設置的過濾器58、流量調整閥60、氣體分析裝置62及次泵64以及演算部66及輸出裝置68,因為與第1實施形態相同。省略說明。In the present embodiment, the
本實施形態中,以適當的時序轉換取入閥54與取入閥56,藉由測量CO氣體濃度,可以確認CO氣體產生的位置依存性。具體而言,由於取得各個位置測量的CO濃度差異,可以切開石英坩堝與黑鉛坩堝的反應產生的CO氣體濃度以及SiO氣體與黑鉛的反應產生的CO氣體濃度。In this embodiment, the
(單結晶矽鑄錠的製造方法)
本發明的實施形態的單結晶矽鑄錠的製造方法,使用上述說明的矽單結晶拉引裝置100、200、300,可以適當實施。於是,一邊參照第1〜3圖,一邊說明本發明一實施形態的單結晶矽鑄錠的製造方法。首先,坩堝16內填充多結晶矽鑄錠等矽原料,在主閥44打開的狀態驅動主泵42,減壓下維持密室10內在Ar氣體等非活性氣體空氣中。此時,坩堝16,為了矽原料不接觸熱遮蔽體22,位於密室10內下方。之後,以加熱器24加熱溶融坩堝16內的矽原料,形成矽融液M。之後,上升坩堝16至拉引開始位置。本說明書中,定義「原料溶融步驟」為從開始加熱器24的加熱的時刻到坩堝上升結束的時刻之期間。原料溶融步驟中,非活性氣體的流量以10〜400L(升)/分為佳。(Manufacturing method of single crystal silicon ingot)
The method of manufacturing a single crystal silicon ingot according to an embodiment of the present invention can be suitably implemented using the silicon single
其次,線升降機構32降下拉引線30,使種晶S接觸矽融液M。之後,一邊往既定方向旋轉坩堝16及拉引線30,一邊往上方提拉拉引線30,在種晶S下方生長鑄錠I。又,隨著鑄錠I的生長,雖然矽融液M的量減少,但坩堝16上升,維持融液面的水平。本說明書中,定義「結晶生長步驟」為從開始降下拉引線30的時刻到鑄錠I的生長(拉引線30的上升)結束的時刻之期間。
Next, the
結晶生長步驟中,首先因為無錯位化單結晶,進行dash(突進)法的種晶縮小(頸縮),形成頸部In。其次,為了得到必需直徑的鑄錠,生長肩部Is,即使矽單結晶成為所希望的直徑也以一定的直徑生長直幹部Ib。生長直幹部Ib至既定長度後,無錯位的狀態下為了從矽融液M切離單結晶,進行尾部縮小(尾部的形成)。本說明書中,直幹部Ib的生長期間稱作「直幹步驟」。 Crystal growth step, firstly because of the dislocation-free single crystal, a Dash (plunging) seeding reduction method (necking), forming a neck I n. Secondly, in order to obtain an ingot of the necessary diameter, the shoulder portion I s is grown, and the straight stem portion I b is grown with a certain diameter even if the silicon single crystal becomes the desired diameter. After the straight stem I b is grown to a predetermined length, in order to cut the single crystal from the silicon melt M without dislocation, the tail is reduced (the formation of the tail). In this specification, the growth period of the straight stem portion I b is referred to as the "straight stem step".
結晶生長步驟中,非活性氣體的流量以50~300L/分為佳。又,結晶生長步驟中,非活性氣體的流量,在上述範圍內隨著時間增減(變動)。 In the crystal growth step, the flow rate of the inert gas is preferably 50~300L/min. In addition, in the crystal growth step, the flow rate of the inert gas increases or decreases (varies) with time within the above-mentioned range.
本實施形態中,特徵在於原料溶融步驟及結晶生長步驟中進行以下步驟。首先採集爐內氣體。此步驟,如第1~3圖所示,從氣體採集口46及氣體採集口48的一方或兩方,透過吸引爐內氣體至次配管52進行。
This embodiment is characterized in that the following steps are performed in the raw material melting step and the crystal growth step. First collect the gas in the furnace. This step is performed by sucking the gas in the furnace to the
其次,以氣體分析裝置62間歇測量採集的氣體中的CO氣體濃度。於是,演算部66,透過將測量的CO氣體濃度乘以供給至密室10內的非活性氣體流量,算出CO氣體產生率。於是,輸出裝置68輸出算出的CO氣體產生率。本實施形態中,代替爐內氣體的CO氣體濃度,可以即時監視爐內氣體的CO氣體產生率。這樣,由於現場(in-situ)監視CO氣體產生率,可以適當評估不僅矽融液內CO氣體的取入量甚至結晶中的碳濃度。又,如同既述,供給至密室10內的非活性氣體流量,在原料溶融步驟與結晶生長步驟中不同,又,結晶生長步驟中即使變動,只要使用監視時的氣體流量設定值即可。
Next, the
本實施形態中,原料溶融步驟中CO氣體產生率最大值為A(mol/h),結晶生長步驟的直幹步驟中CO氣體產生率最大值為B(mol/h),原料溶融步驟及結晶生長步驟,理想是在滿足A/B≦10的條件下進行。滿足A/B≦10的條件下,可以製造結晶固化率在0.75以下的全部位中碳濃度(Cs)為2×1015 atom/cm3 (原子/立方厘米)以下的單結晶矽鑄錠。即,可以高成品率製造碳濃度低的單結晶矽鑄錠。又,結晶固化率(%),以提拉中的結晶質量/原料的加入質量百分率定義。又,原料溶融步驟中最初的10小時,由於密室內從元件脫離的氣體,CO氣體產生率不穩定。於是,本說明書中,採用原料溶融步驟中除去初期的10小時的期間的最大值作為A。In this embodiment, the maximum CO gas generation rate in the raw material melting step is A (mol/h), the maximum CO gas generation rate in the direct drying step of the crystal growth step is B (mol/h), the raw material melting step and crystal growth The step is ideally performed under the condition that A/B≦10 is satisfied. Under the condition of A/B≦10, it is possible to produce single crystal silicon ingots with a solidification rate of less than 0.75 and a carbon concentration (C s ) of 2×10 15 atom/cm 3 (atoms/cubic centimeter) or less in all positions. . That is, a single crystal silicon ingot with a low carbon concentration can be manufactured at a high yield. In addition, the crystal solidification rate (%) is defined by the crystal mass during pulling/the added mass percentage of the raw material. Also, during the first 10 hours of the raw material melting step, the CO gas generation rate was unstable due to the gas detached from the element in the closed chamber. Therefore, in this specification, the maximum value during the initial 10-hour period of removal in the raw material melting step is taken as A.
A/B值,主要透過控制原料溶融步驟中加熱器24的電能可以調節。一般,結晶生長步驟中,維持矽融液M需要的加熱器24的電能由本身與既定範圍值決定,以上述特定的電能驅動加熱器維持矽融液M。因此,結晶生長步驟中的CO氣體產生率比較低且穩定(沒有大變動)。相對於此,原料溶融步驟中,為了溶融矽原料需要以大電能驅動加熱器24,CO氣體產生率比較高且不穩定(大變動)。尤其,原料溶融步驟的末期(溶融結束時),CO氣體產生率有變大的傾向。於是,控制原料溶融步驟中的加熱器24的電能,藉由抑制CO氣體產生率最大值A,可以實現A/B≦10。但是,A和B的值,不是唯一根據加熱器24的電能決定,也依存於密室10內的斷熱性(即,密室的構造、斷熱體的量和配置)。The A/B value can be adjusted mainly by controlling the electric energy of the
A/B是1以上為佳。因為,A/B未達1時,矽融液固化,結晶生長恐怕不成立。 [實施例]A/B is preferably 1 or more. This is because when A/B is less than 1, the silicon melt solidifies and crystal growth may not be established. [Example]
(實驗例1) 使用第1圖所示構成的矽單結晶拉引裝置,以表1所示的4水準進行單結晶矽鑄錠的製造。各水準都是矽原料的裝載量320Kg(公斤)、鑄錠的直徑300mm(毫米)、直幹長1800mm 、生長速度1.0mm/分,原料溶融步驟中供給至密室內的Ar氣體流量為100L/分。使用可以除去粒徑1μm以上的粒子99質量%以上之具有奈米級的網目尺寸的氣體過濾器。原料溶融步驟及結晶生長步驟中的加熱器電能為表1所示的值。(Experimental example 1) Using the silicon single crystal pulling device configured as shown in Fig. 1, single crystal silicon ingots were manufactured at the four levels shown in Table 1. For each level, the loading capacity of silicon raw material is 320Kg (kg), the diameter of the ingot is 300mm (mm), the straight stem length is 1800mm, and the growth rate is 1.0mm/min. The flow rate of Ar gas supplied to the chamber during the raw material melting step is 100L/min. . Use a gas filter with a nano-level mesh size that can remove 99% by mass or more of particles with a particle size of 1 μm or more. The heater electric energy in the raw material melting step and the crystal growth step is the value shown in Table 1.
作為氣體分析裝置使用四層極型質量分析裝置,原料溶融步驟及結晶生長步驟的全過程中,監視CO氣體產生率。表1中顯示原料溶融步驟中的CO氣體產生率最大值A及直幹步驟中的CO氣體產生率最大值B。又,第5圖中顯示,代表全水準,以水準No.1顯示監視的CO氣體產生率的推移。 A four-layer polar mass analyzer is used as a gas analyzer, and the CO gas generation rate is monitored during the entire process of the raw material melting step and the crystal growth step. Table 1 shows the maximum value A of the CO gas generation rate in the raw material melting step and the maximum value B of the CO gas generation rate in the direct drying step. In addition, the display in Figure 5 represents the full level, and level No. 1 shows the transition of the monitored CO gas generation rate.
各水準中,根據以下的程序求出表1中所示的「低碳結晶成品率」。首先,從各水準製造的單結晶矽鑄錠的直幹部切出,加工製造多枚矽晶圓。在各晶圓的中心1點,使用FT-IR裝置測量矽的結晶位置中置換的碳濃度(Cs)。對於生長的結晶長為分母,滿足Cs≦2×1015atoms/cm3以下的結晶長為分子,求出結晶成品率,成為「低碳結晶成品率」。表1中顯示結果。 For each level, the "low-carbon crystal yield" shown in Table 1 was obtained according to the following procedure. First, cut out the straight stems of single crystal silicon ingots manufactured at various levels, and process and manufacture multiple silicon wafers. At one point in the center of each wafer, the FT-IR device was used to measure the carbon concentration (Cs) substituted in the silicon crystal position. Regarding the growth of the crystal length as the denominator, the crystal length satisfying Cs≦2×10 15 atoms/cm 3 or less is the numerator, and the crystal yield is determined to be the "low carbon crystal yield". The results are shown in Table 1.
如同表1很清楚地,滿足A/B≦10的條件下實行水準No.1~4中對於低碳結晶成品率75%以上與高位,A/B=11的條件下實行的水準No.5中,低碳結晶成品率25%明顯下降。 As shown in Table 1, it is clear that the implementation level No. 1 to 4 under the condition of A/B≦10 is the level No. 5 implemented under the condition of A/B=11 for low-carbon crystal yields of 75% or more and high. The yield rate of medium and low-carbon crystals dropped significantly by 25%.
(實驗例2) (Experimental example 2)
依存於氣體過濾器的性能和有無,測量次配管(具體而言,流量調整閥、流量調整閥與氣體分析裝置之間)不堵塞可連續監視CO氣體產生率的時間。單結晶矽鑄錠的製造方法,除了過濾器以外與實驗例1相同。 Depending on the performance and presence of the gas filter, the measurement of the time during which the secondary piping (specifically, the flow adjustment valve, the flow adjustment valve, and the gas analysis device) is not clogged and the CO gas generation rate can be continuously monitored. The manufacturing method of the single crystal silicon ingot was the same as in Experimental Example 1 except for the filter.
水準1,與實驗例1相同,使用可以除去粒徑1μm以上的粒子99質量%以上之具有奈米級的網目尺寸的氣體過濾器。此水準1中,可連續100小時以上監視CO氣體產生率。
水準2,使用具有可以除去粒徑10μm以上的粒子99質量%以上之網目尺寸的氣體過濾器。此水準2中,即使連續70小時以上進行監視CO氣體產生率,次配管也堵塞,不能監視。Level 2, using a gas filter with a mesh size that can remove 99% by mass or more of particles with a particle size of 10 μm or more. In this level 2, even if the CO gas generation rate is monitored continuously for more than 70 hours, the secondary piping is clogged and cannot be monitored.
水準3,不使用氣體過濾器。此水準2中,即使連續20小時以上進行監視CO氣體產生率,次配管也堵塞,不能監視。 [產業上的利用可能性]Level 3, no gas filter is used. In this level 2, even if the CO gas generation rate is monitored continuously for more than 20 hours, the secondary piping is clogged and cannot be monitored. [Industrial Utilization Possibility]
根據本發明的單結晶矽鑄錠的製造方法及矽單結晶拉引裝置,可以高成品率製造碳濃度低的單結晶矽鑄錠。According to the method for manufacturing a single crystal silicon ingot and the silicon single crystal pulling device of the present invention, a single crystal silicon ingot with a low carbon concentration can be manufactured at a high yield.
10:密室
12:氣體導入口
14:氣體排出口
16:坩堝
16A:石英坩堝
16B:黑鉛坩堝
18:傳動軸
20:軸驅動機構
22:熱遮蔽體
22A:遮蔽本體
22B:內側凸緣部
22C:外側凸緣部
24:加熱器
26:斷熱體
28:種晶夾頭
30:拉引線
32:線升降機構
34:開口部
36:CCD攝影機
40:排氣配管
42:主泵
44:主閥
46:氣體採集口(排氣配管)
48:氣體採集口(密室內)
50:取樣管(密室內)
52:次配管
52A:次配管終端
54:取入閥
56:取入閥
58:過濾器
60:流量調整閥
62:氣體分析裝置
64:次泵
66:演算部
68:輸出裝置
100、200、300、400:矽單結晶拉引裝置
I:單結晶矽鑄錠
In:頸部
Is:肩部
Ib:直幹部
M:矽融液
S:種晶
X:拉引軸10: Secret Chamber
12: Gas inlet
14: Gas outlet
16:
[第1圖]係概要顯示本發明第1實施形態的矽單結晶拉引裝置100構成之沿著拉引軸X的剖面圖;
[第2圖]係概要顯示本發明第2實施形態的矽單結晶拉引裝置200構成之沿著拉引軸X的剖面圖;
[第3圖]係概要顯示本發明第3實施形態的矽單結晶拉引裝置300構成之沿著拉引軸X的剖面圖;
[第4圖]係概要顯示習知的矽單結晶拉引裝置400構成之沿著拉引軸X的剖面圖;
[第5圖]係在No.1(第1號)的原料溶融步驟及結晶生長步驟中CO氣體產生率的推移圖表;以及
[第6圖]係從密室內採集的氣體中的SiO粉末顆粒大小分布圖表。[Figure 1] is a cross-sectional view along the pulling axis X schematically showing the structure of the silicon single
10:密室 10: Secret Chamber
12:氣體導入口 12: Gas inlet
14:氣體排出口 14: Gas outlet
16:坩堝 16: Crucible
16A:石英坩堝 16A: Quartz crucible
16B:黑鉛坩堝 16B: Black lead crucible
18:傳動軸 18: drive shaft
20:軸驅動機構 20: Shaft drive mechanism
22:熱遮蔽體 22: Heat shielding body
22A:遮蔽本體 22A: Cover the body
22B:內側凸緣部 22B: Inside flange
22C:外側凸緣部 22C: Outer flange
24:加熱器 24: heater
26:斷熱體 26: Insulating body
28:種晶夾頭 28: Seed chuck
30:拉引線 30: Pull the lead
32:線升降機構 32: Line lifting mechanism
34:開口部 34: Opening
36:CCD攝影機 36: CCD camera
40:排氣配管 40: Exhaust pipe
42:主泵 42: main pump
44:主閥 44: main valve
46:氣體採集口(排氣配管) 46: Gas collection port (exhaust piping)
52:次配管 52: Secondary piping
52A:次配管終端 52A: Secondary piping terminal
58:過濾器 58: filter
60:流量調整閥 60: Flow adjustment valve
62:氣體分析裝置 62: Gas analysis device
64:次泵 64: Secondary pump
66:演算部 66: calculation department
68:輸出裝置 68: output device
100:矽單結晶拉引裝置 100: Silicon single crystal pulling device
I:單結晶矽鑄錠 I: Single crystal silicon ingot
In:頸部 In: neck
Is:肩部 Is: Shoulder
Ib:直幹部 Ib: Straight Officer
M:矽融液 M: Silicon melt
S:種晶 S: seed crystal
X:拉引軸 X: pull shaft
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US5131974A (en) * | 1989-11-16 | 1992-07-21 | Shin-Etsu Handotai Co., Ltd. | Method of controlling oxygen concentration in single crystal and an apparatus therefor |
TWI399465B (en) * | 2009-05-27 | 2013-06-21 | Japan Super Quartz Corp | Method of manufacturing silicon single crystal, apparatus for pulling silicon single crystal and vitreous silica crucible |
US20130277809A1 (en) * | 2010-12-28 | 2013-10-24 | Siltronic Ag | Method of manufacturing silicon single crystal, silicon single crystal, and wafer |
TW201823527A (en) * | 2016-12-02 | 2018-07-01 | 日商Sumco股份有限公司 | method of manufacturing single-crystalline silicon |
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CN113302346B (en) | 2023-11-03 |
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TW202025339A (en) | 2020-07-01 |
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WO2020129330A1 (en) | 2020-06-25 |
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