TW202405262A - Method of obtaining crystal ingot heat history and monocrystal furnace - Google Patents
Method of obtaining crystal ingot heat history and monocrystal furnace Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 277
- 238000000034 method Methods 0.000 title claims abstract description 80
- 238000009529 body temperature measurement Methods 0.000 claims description 72
- 239000007788 liquid Substances 0.000 claims description 50
- 230000008569 process Effects 0.000 claims description 48
- 239000010453 quartz Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 235000014347 soups Nutrition 0.000 claims description 11
- 230000004308 accommodation Effects 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 9
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- 238000001816 cooling Methods 0.000 description 25
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- 238000004519 manufacturing process Methods 0.000 description 8
- 238000004880 explosion Methods 0.000 description 5
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 230000008646 thermal stress Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
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- 238000009792 diffusion process Methods 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000002231 Czochralski process Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- C30—CRYSTAL GROWTH
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C30B15/206—Controlling or regulating the thermal history of growing the ingot
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Abstract
Description
本申請涉及半導體領域，具體地，涉及獲取晶棒熱歷史的方法和單晶爐。The present application relates to the field of semiconductors and, in particular, to methods of obtaining thermal history of crystal ingots and single crystal furnaces.
在直拉法（Czochralski process，簡稱CZ法）單晶爐晶體生長過程中，晶棒的熱歷史直接影響晶體缺陷的擴散、氧沉澱、熱應力等重要參數。因此，監控晶棒的熱歷史是非常有必要的。During the crystal growth process in a single crystal furnace using the Czochralski process (CZ method for short), the thermal history of the crystal rod directly affects important parameters such as the diffusion of crystal defects, oxygen precipitation, and thermal stress. Therefore, it is necessary to monitor the thermal history of the ingot.
因此，目前獲取晶棒熱歷史的方法和單晶爐仍有待改進。Therefore, the current methods of obtaining the thermal history of crystal ingots and single crystal furnaces still need to be improved.
本申請是基於發明人對於以下事實和問題的發現和認識做出的：This application is based on the inventor's discovery and understanding of the following facts and problems:
晶棒的熱歷史直接影響晶體缺陷的擴散、氧沉澱、熱應力等與晶棒性能直接或間接相關的參數。發明人發現，相關技術中通常在CZ法晶爐晶體生長過程中，透過電腦軟體來模擬計算晶棒的冷却過程，並未對晶棒進行冷却速率的實際監控。進一步地，發明人發現，根據電腦軟體模擬得到的晶棒冷却過程中晶棒冷却速率的實際調整，會出現調整結果與模擬結果不一致的情况。因此，電腦軟體模擬得到的晶棒冷却過程與實際冷却過程之間始終存在一定的誤差，從而使得在實際操作中無法直接、準確地調整晶棒的冷却速率，使得晶棒在取棒出爐過程中，會因冷却速率過快導致其內部存在熱應力，進而發生***，或因冷却速率過慢導致晶棒的冷却時間過長，嚴重影響産能。The thermal history of the crystal ingot directly affects the diffusion of crystal defects, oxygen precipitation, thermal stress and other parameters that are directly or indirectly related to the performance of the crystal ingot. The inventor found that in the related art, during the crystal growth process of the CZ crystal furnace, computer software is usually used to simulate and calculate the cooling process of the crystal rod, but the cooling rate of the crystal rod is not actually monitored. Further, the inventor found that according to the actual adjustment of the crystal rod cooling rate during the crystal rod cooling process simulated by computer software, the adjustment results may be inconsistent with the simulation results. Therefore, there is always a certain error between the cooling process of the crystal ingot simulated by computer software and the actual cooling process, which makes it impossible to directly and accurately adjust the cooling rate of the crystal ingot in actual operations. , the cooling rate will be too fast, resulting in thermal stress inside the ingot, which will lead to an explosion, or the cooling rate will be too slow, causing the cooling time of the ingot to be too long, seriously affecting production capacity.
本申請旨在至少一定程度上緩解或解決上述提及問題中至少一個。The present application aims to alleviate or solve at least one of the above-mentioned problems to at least a certain extent.
在本申請的一個方面，本申請提出了一種獲取長晶過程中晶棒熱歷史的方法，包括：步驟S1：確定晶棒的待測溫橫截面。步驟S2：令晶種接觸熔湯液面後，垂直提拉晶種以長晶獲得晶棒，並在初始時間點開始計時，初始時間點標記為t 0。步驟S3：在長晶過程中，透過多個紅外測溫裝置依次獲取待測溫橫截面的溫度，並標示待測溫橫截面的溫度為T x，並依次記錄多個紅外測溫裝置測得待測溫橫截面的溫度時的時間點，並標示測得待測溫橫截面的溫度時的時間點為t x，其中，x為大於等於1的正整數，x的最大值等於紅外測溫裝置的數量。步驟S4：在坐標系中，以測得待測溫橫截面的溫度時的時間點t x為橫坐標、待測溫橫截面的溫度T x為縱坐標獲得多個坐標點，依次連接多個坐標點以獲取長晶過程中晶棒熱歷史曲線。由此，可以獲得實際的晶棒熱歷史曲線。 In one aspect of this application, this application proposes a method for obtaining the thermal history of a crystal rod during the crystal growth process, including: Step S1: Determine the temperature cross-section of the crystal rod to be measured. Step S2: After the seed crystal contacts the molten liquid surface, pull the seed crystal vertically to grow the crystal to obtain a crystal rod, and start timing at the initial time point, which is marked as t 0 . Step S3: During the crystal growth process, obtain the temperature of the cross-section to be measured through multiple infrared temperature measurement devices in sequence, mark the temperature of the cross-section to be measured as T x , and record the values measured by the multiple infrared temperature measurement devices in sequence. The time point when the temperature of the cross-section to be measured is measured, and the time point when the temperature of the cross-section to be measured is measured is t x , where x is a positive integer greater than or equal to 1, and the maximum value of x is equal to the infrared temperature measurement Number of devices. Step S4: In the coordinate system, use the time point t x when the temperature of the cross-section to be measured is measured as the abscissa, and the temperature T x of the cross-section to be measured as the ordinate to obtain multiple coordinate points, and connect multiple coordinate points to obtain the thermal history curve of the crystal rod during the crystal growth process. From this, the actual thermal history curve of the ingot can be obtained.
根據本申請的實施例，步驟S1進一步包括：確定待測溫橫截面，待測溫橫截面為晶棒的等徑長度為設定值時所在的橫截面。步驟S2進一步包括：令晶種接觸熔湯液面後，垂直提拉晶種以獲得晶棒，當熔湯液面上的晶棒等徑長度為設定值時，開始在初始時間點計時，初始時間點標記為t 0。由此，可以獲得晶棒上任一點處的熱歷史曲線。 According to an embodiment of the present application, step S1 further includes: determining a temperature cross-section to be measured, where the temperature cross-section to be measured is the cross-section where the equal diameter length of the crystal rod is at a set value. Step S2 further includes: after making the crystal seed contact the molten liquid surface, pull the seed crystal vertically to obtain the crystal rod. When the equal diameter length of the crystal rod on the molten liquid surface reaches the set value, start timing at the initial time point. The time point is marked t 0 . From this, the thermal history curve at any point on the crystal rod can be obtained.
根據本申請的實施例，步驟S2進一步包括：初始時間點t0開始計時，透過至少一個紅外測溫裝置測量熔湯液面的初始溫度，並標示初始溫度為T 0。步驟S4進一步包括：在坐標系中，以測得待測溫橫截面的溫度時的時間點t x為橫坐標、待測溫橫截面的溫度T x為縱坐標獲得多個坐標點，在坐標系中，以初始時間點t 0為橫坐標、初始溫度T 0為縱坐標獲得起始坐標點，依次連接起始坐標點和多個坐標點，以獲取長晶過程中的晶棒熱歷史曲線。由此，可以獲得實際的晶棒熱歷史曲線。 According to the embodiment of the present application, step S2 further includes: starting timing from the initial time point t0, measuring the initial temperature of the molten liquid surface through at least one infrared temperature measuring device, and marking the initial temperature as T 0 . Step S4 further includes: in the coordinate system, using the time point t x when the temperature of the cross-section to be measured is measured as the abscissa and the temperature T x of the cross-section to be measured as the ordinate to obtain multiple coordinate points. In the system, the initial time point t 0 is used as the abscissa and the initial temperature T 0 is used as the ordinate to obtain the starting coordinate point. The starting coordinate point and multiple coordinate points are connected in sequence to obtain the thermal history curve of the crystal ingot during the crystal growth process. . From this, the actual thermal history curve of the ingot can be obtained.
根據本申請的實施例，步驟S3進一步包括：獲取紅外測溫裝置的測溫點和熔湯液面之間的距離，並標示紅外測溫裝置的測溫點和熔湯液面之間的距離為d x，步驟S4進一步包括：在坐標系中，以紅外測溫裝置的測溫點和熔湯液面之間的距離d x為橫坐標，待測溫橫截面的溫度T x為縱坐標獲得多個坐標點，依次連接多個坐標點以獲取長晶過程中的晶棒熱歷史曲線。由此，可以獲得多種實際的晶棒熱歷史曲線。 According to the embodiment of the present application, step S3 further includes: obtaining the distance between the temperature measurement point of the infrared temperature measurement device and the molten liquid level, and marking the distance between the temperature measurement point of the infrared temperature measurement device and the molten liquid level. is d x , step S4 further includes: in the coordinate system, the distance d x between the temperature measurement point of the infrared temperature measurement device and the melt liquid level is the abscissa, and the temperature T Obtain multiple coordinate points and connect multiple coordinate points in sequence to obtain the thermal history curve of the ingot during the crystal growth process. From this, a variety of actual ingot thermal history curves can be obtained.
根據本申請的實施例，進一步包括：調整單晶爐的熱場，並重複步驟S1~步驟S4；調整單晶爐中的熱場包括以下至少之一：調整導流筒的下邊緣與熔湯液面之間的距離；調整導流筒的材料的隔熱係數；調整垂直提拉晶種的速率；調整加熱器的加熱功率。由此，可以對晶棒熱歷史進行調整。According to the embodiment of the present application, it further includes: adjusting the thermal field of the single crystal furnace, and repeating steps S1 to S4; adjusting the thermal field of the single crystal furnace includes at least one of the following: adjusting the lower edge of the guide tube and the molten soup The distance between the liquid levels; adjust the thermal insulation coefficient of the material of the guide tube; adjust the rate of vertical pulling of the seed crystal; adjust the heating power of the heater. Thus, the thermal history of the ingot can be adjusted.
根據本申請的實施例，進一步包括：步驟S5：調整垂直提拉晶種的速率，並重複步驟S1~步驟S4。由此，可以對晶棒熱歷史進行調整。According to the embodiment of the present application, it further includes: step S5: adjust the rate of vertical pulling of the seed crystal, and repeat steps S1 to S4. Thus, the thermal history of the ingot can be adjusted.
在本申請的另一個方面，本申請提出了一種單晶爐，包括主爐室、石英坩堝以及導流筒。主爐室內限定出容納空間。石英坩堝設在容納空間內以熔化原料且盛放熔湯，石英坩堝上方具有可垂直移動晶種的空間，晶種可垂直移動地設在石英坩堝上方且可伸入熔湯中以便長晶獲得晶棒。導流筒設在容納空間內。其中，單晶爐的側壁上開設有多個透光窗口，多個透光窗口處設置有多個紅外測溫裝置，多個紅外測溫裝置的測溫點的高度不同，多個紅外測溫裝置被配置為：在長晶過程中，可依次對晶棒上的同一橫截面處進行測溫。由此，可以對晶棒生産過程中的熱歷史進行準確監控。In another aspect of this application, this application proposes a single crystal furnace, including a main furnace chamber, a quartz crucible and a guide tube. The accommodation space is limited in the main furnace room. The quartz crucible is placed in the accommodation space to melt the raw materials and hold the molten soup. There is a space above the quartz crucible where the seed crystal can be moved vertically. The seed crystal can be vertically moved above the quartz crucible and can be extended into the molten soup to facilitate crystal growth. crystal rod. The guide tube is located in the accommodation space. Among them, there are multiple light-transmitting windows on the side walls of the single crystal furnace, and multiple infrared temperature measurement devices are installed at the multiple light-transmitting windows. The temperature measurement points of the multiple infrared temperature measurement devices have different heights. The multiple infrared temperature measurement devices The device is configured to measure the temperature of the same cross-section on the crystal rod in sequence during the crystal growth process. This allows the thermal history of the ingot to be accurately monitored during production.
根據本申請的實施例，單晶爐進一步包括：副室。副室的底端與主爐室的爐蓋相連接，主爐室的側壁和/或副室的側壁上開設有多個透光窗口。由此，可以透過簡單的結構設計實現晶棒生産過程中熱歷史的監控。According to an embodiment of the present application, the single crystal furnace further includes: an auxiliary chamber. The bottom end of the auxiliary chamber is connected to the furnace cover of the main furnace chamber, and multiple light-transmitting windows are provided on the side walls of the main furnace chamber and/or the side walls of the auxiliary chamber. As a result, the thermal history monitoring during the ingot production process can be realized through simple structural design.
根據本申請的實施例，至少一個紅外測溫裝置的測溫點與紅外測溫裝置的連線垂直於晶棒的長度方向。由此，便於進行紅外測溫裝置的設置。According to an embodiment of the present application, the connection line between the temperature measurement point of at least one infrared temperature measurement device and the infrared temperature measurement device is perpendicular to the length direction of the crystal rod. This facilitates the installation of the infrared temperature measurement device.
根據本申請的實施例，至少一個紅外測溫裝置被配置為：對石英坩堝中熔湯的液面處進行測溫。由此，便於實現晶棒熱歷史的完整監控。According to an embodiment of the present application, at least one infrared temperature measurement device is configured to measure the temperature of the liquid surface of the molten soup in the quartz crucible. This facilitates complete monitoring of the thermal history of the ingot.
下面詳細描述本申請的實施例，所述實施例的示例在附圖中示出，其中自始至終相同或類似的標號表示相同或類似的元件或具有相同或類似功能的元件。下面透過參考附圖描述的實施例是示例性的，僅用於解釋本申請，而不能理解為對本申請的限制。The embodiments of the present application are described in detail below. Examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements with the same or similar functions. The embodiments described below with reference to the drawings are exemplary and are only used to explain the present application and cannot be understood as limiting the present application.
在本申請的一個方面，本申請提出了一種獲取長晶過程中晶棒熱歷史的方法，透過獲取的熱歷史曲線，可以比較不同長晶過程中的冷却速率差異；透過結合晶棒的性能測試，可以反推得到熱歷史曲線應進行實際改進，進而透過優化單晶爐熱場等參數獲得具有較優熱歷史的高品質晶棒。In one aspect of this application, this application proposes a method for obtaining the thermal history of the crystal rod during the crystal growth process. Through the obtained thermal history curve, the difference in cooling rates in different crystal growth processes can be compared; through the performance test of the combined crystal rod , it can be deduced that the thermal history curve should be actually improved, and then high-quality crystal ingots with better thermal history can be obtained by optimizing parameters such as the thermal field of the single crystal furnace.
根據本申請的一些實施例，本申請中獲取長晶過程中晶棒熱歷史的設備不受特別限制，例如，本申請中獲取方法可以用於單晶爐、真空爐等設備長晶過程中的晶棒熱歷史獲取。下面以單晶爐為例，對於前述獲取長晶過程中晶棒熱歷史的方法進行說明：According to some embodiments of the present application, the equipment for obtaining the thermal history of the crystal rod during the crystal growth process in this application is not particularly limited. For example, the acquisition method in this application can be used in the crystal growth process of single crystal furnaces, vacuum furnaces and other equipment. Ingot thermal history acquisition. Taking a single crystal furnace as an example, the following method will be used to explain the aforementioned method of obtaining the thermal history of the crystal rod during the crystal growth process:
具體地，參考圖3，獲取單晶爐長晶過程中晶棒熱歷史的方法包括以下步驟：Specifically, referring to Figure 3, the method of obtaining the thermal history of the crystal rod during the crystal growth process in a single crystal furnace includes the following steps:
步驟S1：確定晶棒的待測溫橫截面Step S1: Determine the temperature cross-section of the crystal rod to be measured
根據本申請的一些實施例，在步驟S1確定晶棒的待測溫橫截面，從而可以在長晶過程中，透過多個紅外測溫裝置依次對晶棒上的同一橫截面處進行測溫，準確監控晶棒。According to some embodiments of the present application, the cross-section of the crystal rod to be measured is determined in step S1, so that during the crystal growth process, the temperature of the same cross-section on the crystal rod can be measured sequentially through multiple infrared temperature measurement devices, Accurately monitor crystal ingots.
根據本申請的一些實施例，確定晶棒的待測溫橫截面的方法不受特別限制，例如，步驟S1可以進一步包括：確定待測溫橫截面，待測溫橫截面為晶棒的等徑長度為設定值時所在的橫截面，即處於晶棒等徑長度在設定值時位置的橫截面，設定值標示為L。可以理解的是，自晶種接觸熔湯液面後進行長晶過程中，依次經過縮徑階段、放肩階段、等徑階段以及收尾階段，等徑長度為晶棒直徑達到預設直徑開始起算的長度，如預設直徑為300mm，則當晶棒直徑達到300mm開始起算等徑長度。舉例來說，設定預設直徑為300mm以及晶棒的等徑長度為設定值L=400mm時所在的橫截面為待測溫橫截面，其含義是從等徑長度的起算點為晶棒直徑剛達到300mm的位置，距起算點的長度為400mm時的待測溫橫截面。以目標晶棒的等徑長度為2800mm為例，可以測量待測部分長度為0~2800mm範圍內的任意一值時所在晶棒橫截面處的溫度在長晶過程中的變化，具體地，待測部分長度（即設定值L）可以為500mm、1000mm、1500mm、2000mm以及2500mm等值，故透過選用不同的等徑長度處做為晶棒的待測溫橫截面，對晶棒等徑長度處各個位置點熱歷史均可實現精準監控。According to some embodiments of the present application, the method of determining the temperature cross-section of the crystal rod to be measured is not particularly limited. For example, step S1 may further include: determining the temperature cross-section to be measured, and the temperature cross-section to be measured is the equal diameter of the crystal rod. The length is the cross section where the set value is, that is, the cross section where the equal diameter length of the crystal rod is at the set value. The set value is marked L. It can be understood that during the crystal growth process after the crystal seed contacts the molten liquid surface, it goes through the diameter reduction stage, the shoulder release stage, the equal diameter stage and the finishing stage. The equal diameter length is calculated from when the diameter of the crystal rod reaches the preset diameter. The length, if the preset diameter is 300mm, the equal diameter length will be calculated when the diameter of the crystal rod reaches 300mm. For example, when the preset diameter is set to 300mm and the equal diameter length of the crystal rod is the set value L=400mm, the cross section is the temperature cross section to be measured. This means that the starting point of the equal diameter length is the diameter of the crystal rod. The temperature cross-section to be measured reaches the position of 300mm and the length from the starting point is 400mm. Taking the equal diameter length of the target crystal rod as 2800mm as an example, the temperature change at the cross-section of the crystal rod during the crystal growth process can be measured when the length of the part to be measured is any value within the range of 0~2800mm. Specifically, when The length of the measured part (i.e. the set value L) can be 500mm, 1000mm, 1500mm, 2000mm and 2500mm. Therefore, by selecting different equal diameter lengths as the temperature cross-section of the crystal rod to be measured, the equal diameter length of the crystal rod The thermal history of each location can be accurately monitored.
步驟S2：令晶種接觸熔湯液面後，垂直提拉晶種，並開始計時。Step S2: After the seed crystal contacts the molten liquid surface, pull the seed crystal vertically and start timing.
根據本申請的一些實施例，在步驟S2令晶種接觸熔湯液面後，垂直提拉晶種以獲得晶棒，並在初始時間點開始計時，初始時間點標記為t 0。 According to some embodiments of the present application, after the seed crystal is brought into contact with the molten liquid surface in step S2, the seed crystal is pulled vertically to obtain the crystal rod, and timing is started at an initial time point, which is marked as t 0 .
根據本申請的一些實施例，當確定待測溫橫截面處於晶棒等徑階段長度設定值L時，相應地，步驟S2進一步包括：在令晶種接觸熔湯液面後，垂直提拉晶種以獲得晶棒，其中，當熔湯液面上的晶棒等徑長度為設定值時，再從初始時間點開始進行計時，初始時間點標記為t 0，從而可以精準監控晶棒等徑長度為設定值L的待測溫橫截面在生長過程中的溫度變化。初始時間點t 0不受特別限制，其僅用於表示熱歷史曲線的起始時間點，例如，初始時間點t 0可以為0或大於0的數值。 According to some embodiments of the present application, when it is determined that the temperature cross-section to be measured is at the crystal rod equal diameter stage length setting value L, correspondingly, step S2 further includes: after making the crystal seed contact the molten liquid surface, vertically pulling the crystal method to obtain the crystal rod. When the equal diameter length of the crystal rod on the molten liquid surface reaches the set value, timing is started from the initial time point. The initial time point is marked as t 0 , so that the equal diameter of the crystal rod can be accurately monitored. The temperature change of the cross-section to be measured whose length is the set value L during the growth process. The initial time point t 0 is not particularly limited and is only used to represent the starting time point of the thermal history curve. For example, the initial time point t 0 may be 0 or a value greater than 0.
根據本申請的一些實施例，為了進一步精準監控晶棒生長過程中的熱歷史，可令一個紅外測溫裝置實時測量熔湯液面的溫度，步驟S2進一步包括：當令晶種接觸熔湯液面後，垂直提拉晶種，並開始計時，透過至少一個紅外測溫裝置測量熔湯液面的初始溫度，並標示初始溫度為T 0。由此，可以獲得晶棒的熱歷史曲線的起始坐標點（t 0，T 0）。 According to some embodiments of the present application, in order to further accurately monitor the thermal history of the crystal rod during the growth process, an infrared temperature measurement device can be used to measure the temperature of the molten liquid surface in real time. Step S2 further includes: when the seed crystal contacts the molten liquid surface Then, pull up the seed crystal vertically, start timing, measure the initial temperature of the molten liquid surface through at least one infrared temperature measuring device, and mark the initial temperature as T 0 . From this, the starting coordinate point (t 0 , T 0 ) of the thermal history curve of the crystal rod can be obtained.
步驟S3：在長晶過程中，透過多個紅外測溫裝置依次獲取待測溫橫截面的溫度，並標示待測溫橫截面的溫度為T x，並依次記錄多個紅外測溫裝置測得待測溫橫截面的溫度時的時間點，並標示測得待測溫橫截面的溫度時的時間點為t x。 Step S3: During the crystal growth process, obtain the temperature of the cross-section to be measured through multiple infrared temperature measurement devices in sequence, mark the temperature of the cross-section to be measured as T x , and record the values measured by the multiple infrared temperature measurement devices in sequence. The time point when the temperature of the cross-section to be measured is measured, and the time point when the temperature of the cross-section to be measured is measured is t x .
根據本發明的一些實施例，在步驟S3透過多個紅外測溫裝置（如圖2中示出的紅外測溫裝置T0、T1、T2、T3等紅外測溫裝置）依次獲取待測溫橫截面的溫度，並標示待測溫橫截面的溫度為T x，並依次記錄多個紅外測溫裝置測得待測溫橫截面的溫度時的時間點，並標示測得待測溫橫截面的溫度時的時間點為t x。具體地，參考圖2和圖5，以紅外測溫裝置T0用於測量熔湯液面的初始溫度T 0，紅外測溫裝置T1、T2、T3等紅外測溫裝置用於依次測量晶棒直拉過程中同一橫截面處的溫度為例，以初始時間點t 0時熔湯液面上的晶棒等徑長度在設定值L處的截面P為待測溫橫截面（即P點所在的晶棒水平截面）。在初始時間點t 0時，晶棒等徑長度在設定值L處截面P處於液面位置，此時截面P處的初始溫度為T 0；在時間點t 1時，晶棒等徑長度為L+d 1，此時紅外測溫裝置T1顯示的溫度即為截面P在時間點t 1時，由溫度T 0降為T 1；在時間點t 2時，晶棒等徑長度為L+d 1+d 2，此時紅外測溫裝置T2顯示的溫度即為截面P在時間點t 2時，由溫度T 1降為T 2。以此類推，當截面P依次經過多個紅外測溫裝置測溫後，即可獲得（t 0，T 0）以及多個（t x，T x），從而即可獲得完整的晶棒熱歷史時間和溫度曲線，其中，x為大於等於1的正整數，x的最大值等於紅外測溫裝置的數量。 According to some embodiments of the present invention, in step S3, the temperature cross-section to be measured is sequentially obtained through multiple infrared temperature measurement devices (infrared temperature measurement devices T0, T1, T2, T3 and other infrared temperature measurement devices as shown in Figure 2). the temperature of the cross-section to be measured, and mark the temperature of the cross-section to be measured as T The time point when is t x . Specifically, with reference to Figures 2 and 5, the infrared temperature measuring device T0 is used to measure the initial temperature T 0 of the molten liquid level, and the infrared temperature measuring devices T1, T2, T3 and other infrared temperature measuring devices are used to measure the crystal rod diameter in sequence. Taking the temperature at the same cross-section during the pulling process as an example, take the cross-section P at the set value L of the equal diameter length of the crystal rod on the molten liquid surface at the initial time point t 0 as the temperature cross-section to be measured (that is, where the P point is located) Crystal rod horizontal section). At the initial time point t 0 , the equal diameter length of the crystal rod is at the liquid level at the set value L, and the initial temperature at the cross section P is T 0 ; at the time point t 1 , the equal diameter length of the crystal rod is L+d 1. At this time, the temperature displayed by the infrared temperature measuring device T1 is the cross-section P. At the time point t 1 , the temperature drops from T 0 to T 1 ; at the time point t 2 , the equal diameter length of the crystal rod is L+ d 1 + d 2 , at this time, the temperature displayed by the infrared temperature measuring device T2 is the cross-section P. At time point t 2 , the temperature drops from T 1 to T 2 . By analogy, when the cross-section P is measured by multiple infrared temperature measurement devices in sequence, (t 0 , T 0 ) and multiple (t x , T x ) can be obtained, so that the complete thermal history of the crystal rod can be obtained Time and temperature curve, where x is a positive integer greater than or equal to 1, and the maximum value of x is equal to the number of infrared temperature measuring devices.
根據本申請的一些實施例，步驟S3進一步包括：在長晶過程中，獲取紅外測溫裝置的測溫點和熔湯液面之間的距離，並標示紅外測溫裝置的測溫點和熔湯液面之間的距離為d x，並記錄待測溫橫截面依次經過多個紅外測溫裝置的時間點，並標示測得待測溫橫截面的溫度時的時間點為t x。具體地，參考圖2和圖5，以紅外測溫裝置T0用於測量熔湯液面的溫度T 0，紅外測溫裝置T1、T2、T3等紅外測溫裝置用於依次測量晶棒提拉過程中同一橫截面處的溫度為例，以初始時間點t 0時熔湯液面上的晶棒等徑長度在設定值L處的截面P為待測溫橫截面。在初始時間點t 0時，晶棒等徑長度在設定值L處的截面P位於液面位置，此時晶棒等徑長度為L，d 0=0，初始溫度為T 0；在時間點t 1時，截面P上升d 1，對應晶棒等徑長度L+d 1，待測溫橫截面的溫度為T 1；在時間點t 2時，截面P上升d 1+d 2，對應晶棒等徑長度為L+d 1+d 2，待測溫橫截面的溫度為T 2。以此類推，當截面P依次經過多個紅外測溫裝置測溫後，即可獲得（t 0，d 0）以及多個（t x，d x），從而即可獲得完整的晶棒熱歷史時間和長度變化曲線，其中，x為大於等於1的正整數，x的最大值等於紅外測溫裝置的數量。由此，可以透過改變晶棒提拉速率，進而改變經過相同時間後截面P的上升高度，繼而改變相同時刻對應的晶棒等徑長度，最終透過晶棒提拉速率的改變獲得多條晶棒熱歷史曲線，實現晶棒長晶過程中的熱歷史的調整。 According to some embodiments of the present application, step S3 further includes: during the crystal growth process, obtaining the distance between the temperature measurement point of the infrared temperature measurement device and the melt liquid level, and marking the temperature measurement point of the infrared temperature measurement device and the melt liquid level. The distance between the soup liquid surfaces is d x , and the time point when the cross-section to be measured passes through multiple infrared temperature measurement devices in sequence is recorded, and the time point when the temperature of the cross-section to be measured is measured is marked as t x . Specifically, with reference to Figures 2 and 5, the infrared temperature measuring device T0 is used to measure the temperature T 0 of the molten liquid level, and the infrared temperature measuring devices T1, T2, T3 and other infrared temperature measuring devices are used to measure the crystal rod pulling in sequence. The temperature at the same cross-section during the process is taken as an example. The cross-section P where the equal diameter length of the crystal rod on the molten liquid surface at the initial time point t0 is at the set value L is the cross-section to be measured. At the initial time point t 0 , the section P with the equal diameter length of the crystal rod at the set value L is located at the liquid level. At this time, the equal diameter length of the crystal rod is L, d 0 =0, and the initial temperature is T 0 ; at the time point At time t 1 , the cross-section P rises by d 1 , corresponding to the equal diameter length of the crystal rod L+d 1 , and the temperature of the cross-section to be measured is T 1 ; at time point t 2 , the cross-section P rises by d 1 + d 2, corresponding to the crystal rod's equal diameter length L+d 1 . The equal diameter length of the rod is L+d 1 +d 2 , and the temperature of the cross-section to be measured is T 2 . By analogy, when the cross-section P is measured by multiple infrared temperature measurement devices in sequence, (t 0 , d 0 ) and multiple (t x , d x ) can be obtained, so that the complete thermal history of the crystal rod can be obtained Time and length change curve, where x is a positive integer greater than or equal to 1, and the maximum value of x is equal to the number of infrared temperature measurement devices. Therefore, by changing the pulling rate of the crystal rod, the rising height of the cross-section P after the same time is changed, and then the equal diameter length of the crystal rod corresponding to the same time is changed, and finally multiple crystal rods are obtained by changing the pulling rate of the crystal rod. The thermal history curve realizes the adjustment of the thermal history during the crystal growth process of the crystal ingot.
S4：在坐標系中，以測得待測溫橫截面的溫度時的時間點t x為橫坐標、待測溫橫截面的溫度T x為縱坐標獲得多個坐標點，依次連接多個坐標點。 S4: In the coordinate system, take the time point t x when the temperature of the cross-section to be measured is measured as the abscissa, and the temperature T point.
根據本申請的一些實施例，在步驟S4中，以測得待測溫橫截面的溫度時的時間點t x為橫坐標、待測溫橫截面的溫度T x為縱坐標獲得多個坐標點，依次連接多個坐標點繪製曲線，以獲取長晶過程中的晶棒熱歷史曲線。 According to some embodiments of the present application, in step S4, multiple coordinate points are obtained using the time point t x when the temperature of the cross-section to be measured is measured as the abscissa and the temperature T x of the cross-section to be measured as the ordinate. , connect multiple coordinate points in sequence to draw a curve to obtain the thermal history curve of the crystal rod during the crystal growth process.
根據本申請的一些實施例，步驟S2可進一步包括：當令晶種接觸熔湯液面後，垂直提拉晶種，並開始計時，透過至少一個紅外測溫裝置測量熔湯液面的初始溫度T 0時。相應地，步驟S4可進一步包括：在坐標系中以測得待測溫橫截面的溫度時的時間點t x為橫坐標、待測溫橫截面的溫度T x為縱坐標獲得多個坐標點，在坐標系中以初始時間點t 0為橫坐標、初始溫度T 0為縱坐標獲得起始坐標點，依次連接起始坐標點和多個坐標點獲取長晶過程中的晶棒熱歷史曲線。由此，可以獲得實際的晶棒熱歷史曲線。 According to some embodiments of the present application, step S2 may further include: when the seed crystal contacts the molten liquid surface, vertically pull the seed crystal, and start timing, and measure the initial temperature T of the molten liquid surface through at least one infrared temperature measuring device. 0 o'clock. Correspondingly, step S4 may further include: obtaining multiple coordinate points in the coordinate system with the time point t x when the temperature of the cross-section to be measured is measured as the abscissa and the temperature T x of the cross-section to be measured as the ordinate. , in the coordinate system, use the initial time point t 0 as the abscissa and the initial temperature T 0 as the ordinate to obtain the starting coordinate point, and then connect the starting coordinate point and multiple coordinate points to obtain the thermal history curve of the ingot during the crystal growth process. . From this, the actual thermal history curve of the ingot can be obtained.
根據本申請的一些實施例，步驟S3可進一步包括：在長晶過程中，獲取紅外測溫裝置的測溫點和熔湯液面之間的距離d x，並依次記錄多個紅外測溫裝置測得待測溫橫截面的溫度時的時間點t x。相應地，步驟S4可進一步包括：在坐標系中，以紅外測溫裝置的測溫點和熔湯液面之間的距離d x為橫坐標，待測溫橫截面的溫度T x為縱坐標獲得多個坐標點，依次連接多個坐標點獲取長晶過程中的晶棒熱歷史曲線。由此，可以獲得多種實際的晶棒熱歷史曲線。 According to some embodiments of the present application, step S3 may further include: during the crystal growth process, obtaining the distance d x between the temperature measurement point of the infrared temperature measurement device and the molten liquid level, and recording multiple infrared temperature measurement devices in sequence The time point t x when the temperature of the cross-section to be measured is measured. Correspondingly, step S4 may further include: in the coordinate system, the distance d x between the temperature measurement point of the infrared temperature measurement device and the melt liquid level is the abscissa, and the temperature T x of the cross-section to be measured is the ordinate Obtain multiple coordinate points and connect multiple coordinate points in sequence to obtain the thermal history curve of the ingot during the crystal growth process. From this, a variety of actual ingot thermal history curves can be obtained.
根據本申請的一些實施例，本申請中獲取晶棒熱歷史的方法不受特別限制。例如，參考圖4，獲取晶棒熱歷史的方法可以進一步包括步驟S5：調整單晶爐的熱場，並重複步驟S1~步驟S4。熱場是實物來決定的溫度場分佈，以單晶爐為例，其中實物為石墨材質的部件（如石墨坩堝、加熱器、導流筒等）和保溫層（如硬氈、軟氈等），熱場還受上述實物的相對位置關係影響。具體地，根據本申請的一些實施例，調整單晶爐中的熱場包括以下至少之一：調整導流筒的下邊緣與熔湯液面之間的距離；調整導流筒的材料的隔熱係數；調整加熱器的加熱功率。由此，可以在透過前述方法獲取晶棒熱歷史曲線後，透過調節單晶爐內的熱場進而有目的地調節晶棒熱歷史，降低長晶過程中産生的本徵缺陷，提高晶棒的品質。According to some embodiments of the present application, the method of obtaining the thermal history of the crystal ingot in the present application is not particularly limited. For example, referring to Figure 4, the method of obtaining the thermal history of the crystal ingot may further include step S5: adjusting the thermal field of the single crystal furnace and repeating steps S1 to S4. Thermal field is the temperature field distribution determined by the physical object. Taking a single crystal furnace as an example, the physical object is graphite components (such as graphite crucible, heater, guide tube, etc.) and insulation layer (such as hard felt, soft felt, etc.) , the thermal field is also affected by the relative position of the above-mentioned physical objects. Specifically, according to some embodiments of the present application, adjusting the thermal field in the single crystal furnace includes at least one of the following: adjusting the distance between the lower edge of the guide tube and the molten liquid level; adjusting the distance between the materials of the guide tube. Thermal coefficient; adjust the heating power of the heater. Therefore, after obtaining the thermal history curve of the crystal ingot through the aforementioned method, the thermal history of the crystal ingot can be adjusted purposefully by adjusting the thermal field in the single crystal furnace to reduce the intrinsic defects generated during the crystal growth process and improve the quality of the crystal ingot. quality.
根據本申請的一些實施例，本申請中獲取晶棒熱歷史的方法不受特別限制。獲取晶棒熱歷史的方法可以進一步包括：調整垂直提拉晶種的速率，並重複步驟S1~步驟S4。由此，可以在透過前述方法獲取晶棒熱歷史曲線後，透過調節提拉速率進而有目的地調節晶棒熱歷史，降低長晶過程中産生的本徵缺陷，提高晶棒的品質。本申請中獲取單晶爐長晶過程中晶棒熱歷史的方法具有以下優點中的至少之一：According to some embodiments of the present application, the method of obtaining the thermal history of the crystal ingot in the present application is not particularly limited. The method of obtaining the thermal history of the crystal rod may further include: adjusting the rate of vertical pulling of the seed crystal, and repeating steps S1 to S4. Therefore, after obtaining the thermal history curve of the crystal ingot through the aforementioned method, the thermal history of the crystal ingot can be adjusted purposefully by adjusting the pulling rate, thereby reducing the intrinsic defects generated during the crystal growth process and improving the quality of the crystal ingot. The method of obtaining the thermal history of the crystal rod during the crystal growth process in the single crystal furnace in this application has at least one of the following advantages:
1、實時精準監控晶棒熱歷史，從而可以在晶棒的生長過程中，準確調節晶棒熱歷史，從而改善晶體缺陷分佈、氧沉澱、熱應力等，提高晶棒的品質。1. Accurately monitor the thermal history of the crystal ingot in real time, so that the thermal history of the crystal ingot can be accurately adjusted during the growth process of the crystal ingot, thereby improving crystal defect distribution, oxygen precipitation, thermal stress, etc., and improving the quality of the crystal ingot.
2、透過將取棒/吊料過程中的提拉速率與晶棒熱歷史以熱歷史曲線的形式進行關聯，可以量化調整取棒/吊料過程中的提拉速率，從而控制晶棒的冷却速率，防止因提拉速率過快發生***，或因提拉速率過慢影響産能。2. By correlating the pulling rate during the rod taking/lifting process with the thermal history of the crystal ingot in the form of a thermal history curve, the pulling rate during the rod taking/lifting process can be quantitatively adjusted to control the cooling of the crystal ingot. speed to prevent explosion due to too fast pulling speed, or impact on production capacity due to too slow pulling speed.
3、可以根據晶棒的熱歷史獲取生長過程中，晶棒等徑階段的任一截面處各時刻與溫度的關係曲線，從而可以有目的地優化熱場，提高晶棒的品質。3. According to the thermal history of the crystal ingot, the relationship curve between each moment and the temperature at any cross-section of the crystal ingot during the growth process can be obtained, so that the thermal field can be purposefully optimized and the quality of the crystal ingot can be improved.
在本申請的另一個方面，本申請提出了一種單晶爐，單晶爐可以滿足前述獲取長晶過程中晶棒熱歷史的方法中所需要的設備要求。具體地，參考圖1和圖2，單晶爐包括主爐室、石英坩堝以及導流筒。主爐室10內限定出容納空間。石英坩堝20設在容納空間內以熔化原料且盛放熔湯，石英坩堝20上方具有可垂直移動晶種的空間，晶種可垂直移動地設在石英坩堝20上方且可伸入熔湯中以便長晶獲得晶棒。導流筒30設在容納空間內，且導流筒30的下邊緣與石英坩堝20中熔湯的液面不接觸。其中，單晶爐的側壁上開設有多個透光窗口，多個透光窗口處設置有多個紅外測溫裝置（如圖1中示出的紅外測溫裝置T1、T2、T3等紅外測溫裝置），多個紅外測溫裝置的測溫點的高度不同，多個紅外測溫裝置被配置為：在晶棒的生長過程中，可依次對晶棒上同一橫截面處進行測溫。採用本申請中的單晶爐進行長晶時，利用紅外測溫裝置監控晶棒熱歷史，可以在晶體生長過程中，對晶棒生産過程中的熱歷史進行準確監控。In another aspect of this application, this application proposes a single crystal furnace. The single crystal furnace can meet the equipment requirements required in the aforementioned method of obtaining the thermal history of a crystal rod during crystal growth. Specifically, referring to Figures 1 and 2, the single crystal furnace includes a main furnace chamber, a quartz crucible and a guide tube. The main furnace chamber 10 defines an accommodation space. The quartz crucible 20 is arranged in the accommodation space to melt the raw materials and hold the molten soup. There is a space above the quartz crucible 20 for vertically movable seed crystals. The seed crystals are vertically movable above the quartz crucible 20 and can be extended into the molten soup to facilitate Grow crystals to obtain crystal rods. The flow guide tube 30 is disposed in the accommodation space, and the lower edge of the flow guide tube 30 does not contact the liquid level of the molten liquid in the quartz crucible 20 . Among them, there are multiple light-transmitting windows on the side walls of the single crystal furnace, and multiple infrared temperature measuring devices are installed at the multiple light-transmitting windows (infrared temperature measuring devices T1, T2, T3 and other infrared measuring devices shown in Figure 1). temperature device), the temperature measurement points of the multiple infrared temperature measurement devices are at different heights, and the multiple infrared temperature measurement devices are configured to: during the growth process of the crystal rod, the temperature of the same cross-section on the crystal rod can be measured in sequence. When using the single crystal furnace in this application to grow crystals, an infrared temperature measurement device is used to monitor the thermal history of the crystal rod, so that the thermal history of the crystal rod production process can be accurately monitored during the crystal growth process.
根據本申請的一些實施例，紅外測溫裝置的位置不受特別限制，例如，參考圖2，當單晶爐進一步包括副室40。副室40的底端與主爐室10的爐蓋相連接時，主爐室10的側壁和/或副室40的側壁上開設有多個透光窗口，多個透光窗口處可以設置多個紅外測溫裝置（如圖2中示出的紅外測溫裝置T0、T1、T2、T3等紅外測溫裝置）。具體地，可以採用耐高溫玻璃部分替換單晶爐爐體的原有金屬材料以形成透光窗口，紅外測溫裝置可以包括紅外測溫儀等。According to some embodiments of the present application, the location of the infrared temperature measurement device is not particularly limited. For example, referring to FIG. 2 , when the single crystal furnace further includes an auxiliary chamber 40 . When the bottom end of the auxiliary chamber 40 is connected to the furnace cover of the main furnace chamber 10, multiple light-transmitting windows can be provided on the side walls of the main furnace chamber 10 and/or the side walls of the auxiliary chamber 40. Multiple light-transmitting windows can be provided. An infrared temperature measurement device (infrared temperature measurement device T0, T1, T2, T3 and other infrared temperature measurement devices shown in Figure 2). Specifically, the original metal material of the single crystal furnace body can be partially replaced with high temperature resistant glass to form a light-transmitting window, and the infrared temperature measurement device can include an infrared thermometer.
根據本申請的一些實施例，紅外測溫裝置測溫角度不受特別限制，例如，參考圖1，可以有至少一個紅外測溫裝置（如圖1中示出的T3、T4、T5）的測溫點與紅外測溫裝置的連線垂直於晶棒的長度方向，從而便於進行紅外測溫裝置的設置，以及計算相鄰紅外測溫裝置測溫點之間的距離。According to some embodiments of the present application, the temperature measurement angle of the infrared temperature measurement device is not particularly limited. For example, referring to Figure 1, there can be at least one infrared temperature measurement device (T3, T4, T5 shown in Figure 1). The connection line between the temperature point and the infrared temperature measuring device is perpendicular to the length direction of the crystal rod, which facilitates the setting of the infrared temperature measuring device and the calculation of the distance between the temperature measuring points of adjacent infrared temperature measuring devices.
根據本申請的一些實施例，紅外測溫裝置測溫角度不受特別限制，例如，參考圖2，可以至少一個紅外測溫裝置（如圖2中示出的T0）被配置為：對石英坩堝20中熔湯的液面處進行測溫，從而可以實現晶棒熱歷史的全程監控，獲得更為完整的冷却速率曲線。According to some embodiments of the present application, the temperature measurement angle of the infrared temperature measurement device is not particularly limited. For example, referring to Figure 2, at least one infrared temperature measurement device (T0 shown in Figure 2) can be configured to: measure the quartz crucible The temperature is measured at the liquid surface of the molten soup in 20 degrees, so that the entire thermal history of the crystal rod can be monitored and a more complete cooling rate curve can be obtained.
本申請中的單晶爐透過在常規CZ單晶爐裝置的主爐室10和/或副室40的側壁上開設多個透光窗口，在多個透光窗口處對應地設置多個紅外測溫裝置，透過多個紅外測溫裝置來測定晶棒直拉生長過程中各處的溫度。依照上述工藝制程，可得到晶棒直拉生長過程中的時間t和溫度T的曲線，透過前述曲線可以直接獲得晶棒的實際冷却速率，從而可以根據該曲線有目的地調節晶棒冷却速率，精準控制熔體的溫度分佈，從而降低晶棒氧含量，改善晶體缺陷分佈，獲得高品質晶棒。The single crystal furnace in this application opens multiple light-transmitting windows on the side walls of the main furnace chamber 10 and/or the auxiliary chamber 40 of the conventional CZ single crystal furnace device, and sets multiple infrared detectors correspondingly at the multiple light-transmitting windows. The temperature device uses multiple infrared temperature measuring devices to measure the temperature at various locations during the Czochralski growth process. According to the above process, the curve of time t and temperature T during the Czochralski growth process of the crystal rod can be obtained. The actual cooling rate of the crystal rod can be directly obtained through the aforementioned curve, so that the cooling rate of the crystal rod can be purposefully adjusted according to the curve. Precisely control the temperature distribution of the melt to reduce the oxygen content of the crystal ingot, improve the crystal defect distribution, and obtain high-quality crystal ingots.
下面透過具體的實施例對本申請的方案進行說明，需要說明的是，下面的實施例僅用於說明本申請，而不應視為限定本申請的範圍。實施例中未注明具體技術或條件的，按照本領域內的文獻所描述的技術或條件或者按照産品說明書進行。所用試劑或儀器未注明生産廠商者，均為可以透過市購獲得的常規産品。The solution of the present application will be described below through specific examples. It should be noted that the following examples are only used to illustrate the present application and should not be regarded as limiting the scope of the present application. If specific techniques or conditions are not specified in the examples, the techniques or conditions described in literature in the field or product instructions will be followed. If the manufacturer of the reagents or instruments used is not indicated, they are all conventional products that can be purchased commercially.
實施例1Example 1
導流筒內部使用硬石墨氈作為隔熱材料，實施例1導流筒的下邊緣與熔湯液面的距離為15mm。晶棒提拉速度為0.65mm/min，單晶爐結構如圖2所示，紅外測溫裝置T0測得熔湯液面的溫度為1420℃，並將此時靠近液面一側的晶棒橫截面作為待測溫橫截面P。經過2小時達到紅外測溫裝置T1的位置，此時測得待測溫截面P的溫度為1100℃，再經過2小時達到紅外測溫裝置T2的位置，此時測得待測溫橫截面P的溫度為1020℃。Hard graphite felt is used as the thermal insulation material inside the flow guide tube. The distance between the lower edge of the flow guide tube and the molten liquid level in Example 1 is 15 mm. The crystal rod pulling speed is 0.65mm/min. The structure of the single crystal furnace is shown in Figure 2. The infrared temperature measuring device T0 measured the temperature of the molten liquid surface to be 1420°C, and the crystal rod on the side close to the liquid surface at this time was The cross section is taken as the temperature cross section P to be measured. After 2 hours, it reaches the position of the infrared temperature measurement device T1. At this time, the temperature of the cross-section P to be measured is measured to be 1100°C. After another 2 hours, it reaches the position of the infrared temperature measurement device T2. At this time, the temperature of the cross-section P to be measured is measured. The temperature is 1020℃.
實施例2：Example 2:
實施例2與實施例1保持一致，實施例2與實施例1之間仍有不同之處，前述不同之處是：導流筒內部使用軟氈作為隔熱材料，紅外測溫裝置T0測得液面溫度1420℃。經過2小時，紅外測溫裝置T1測得待測溫截面P的溫度為1000℃，再經過2小時，紅外測溫裝置T2測得待測溫截面P的溫度920℃。Embodiment 2 is consistent with Embodiment 1. There are still differences between Embodiment 2 and Embodiment 1. The aforementioned differences are: soft felt is used as the heat insulation material inside the guide tube, and the infrared temperature measuring device T0 measures The liquid surface temperature is 1420℃. After 2 hours, the infrared temperature measuring device T1 measured the temperature of the section P to be measured to be 1000°C. After another 2 hours, the infrared temperature measuring device T2 measured the temperature of the section P to be measured to be 920°C.
實施例3：Example 3:
實施例3與實施例1保持一致，實施例3與實施例1仍有不同之處，前述不同之處是：實施例3導流筒的下邊緣與熔湯液面的距離為30mm。紅外測溫裝置T0測得熔湯液面溫度為1420℃，並將此時靠近液面一側的晶棒橫截面作為待測溫橫截面P。經過2小時，紅外測溫裝置T1測得待測溫截面P的溫度為1120℃，再經過2小時，紅外測溫裝置T2測得待測溫橫截面P的溫度為1025℃。Embodiment 3 is consistent with Embodiment 1, but there are still differences between Embodiment 3 and Embodiment 1. The aforementioned difference is that the distance between the lower edge of the flow guide tube and the molten liquid level in Embodiment 3 is 30 mm. The infrared temperature measuring device T0 measured the liquid surface temperature of the melt to be 1420°C, and the cross-section of the crystal rod on the side close to the liquid surface at this time was used as the temperature cross-section P to be measured. After 2 hours, the infrared temperature measuring device T1 measured the temperature of the cross-section P to be measured to be 1120°C. After another 2 hours, the infrared temperature measuring device T2 measured the temperature of the cross-section P to be measured to be 1025°C.
實施例4：Example 4:
單晶爐結構如圖2所示，吊料時，提拉速度為3mm/min，待測溫截面P經5.55小時上升至紅外測溫裝置T5位置，紅外測溫裝置T5的測溫點與提拉方向垂直，紅外測溫裝置T5測得待測溫截面P的溫度為700℃。The structure of the single crystal furnace is shown in Figure 2. When lifting materials, the pulling speed is 3mm/min. The cross-section P to be measured rises to the T5 position of the infrared temperature measurement device after 5.55 hours. The temperature measurement point of the infrared temperature measurement device T5 is the same as the lifting speed. The pulling direction is vertical, and the temperature of the section P to be measured is 700°C measured by the infrared temperature measuring device T5.
提拉速度為5mm/min，待測溫截面P經3小時上升至紅外測溫裝置T5位置，紅外測溫裝置T5的測溫點與提拉方向垂直，紅外測溫裝置T5測得待測溫截面P的溫度為740℃，晶棒發生炸裂，具體地參見附圖10及11中的的炸裂測試曲線。The pulling speed is 5mm/min. The cross-section P to be measured rises to the position T5 of the infrared temperature measuring device after 3 hours. The temperature measuring point of the infrared temperature measuring device T5 is perpendicular to the pulling direction. The temperature to be measured is measured by the infrared temperature measuring device T5. The temperature of section P is 740°C, and the crystal rod explodes. For details, see the explosion test curves in Figures 10 and 11.
實施例5：Example 5:
實施例5與實施例4保持一致，實施例5與實施例4仍有不同之處，前述不同之處是：設定初始提拉速度為3mm/min，以該速度保持2小時後；將提拉速度升至到5mm/min，此時再經過2.1小時後，待測溫截面P升至紅外測溫裝置T5位置，紅外測溫裝置T5測得待測溫截面P的溫度為690℃。Embodiment 5 is consistent with Embodiment 4. There are still differences between Embodiment 5 and Embodiment 4. The aforementioned differences are: setting the initial pulling speed to 3mm/min, and maintaining it at this speed for 2 hours; The speed increased to 5mm/min. After another 2.1 hours, the section P to be measured rose to the T5 position of the infrared temperature measurement device. The infrared temperature measurement device T5 measured the temperature of the section P to be measured to be 690°C.
測試結果表明：實施例1的晶棒熱歷史曲線如圖6所示，實施例1與實施例2的晶棒熱歷史曲線如圖7所示。在實施例1中，由於晶棒冷却能力弱，當拉速不小於0.65 mm/min時，晶棒發生扭曲變形，影響生産效率。實施例2選用隔熱效果更好的導流筒材質，晶棒冷却速率快，晶棒的提拉速率提高到極限拉速0.65mm/min以上，即使達到0.7mm/min，晶棒也未發生扭曲變形。結合實施例1與實施例2可知，透過增强導流筒隔熱能力，晶棒冷却速率增加，有益改善高拉速晶棒變形的問題。The test results show that: the thermal history curve of the crystal ingot of Example 1 is shown in Figure 6, and the thermal history curve of the crystal ingot of Example 1 and Example 2 is shown in Figure 7. In Example 1, due to the weak cooling ability of the crystal rod, when the pulling speed is not less than 0.65 mm/min, the crystal rod will be twisted and deformed, affecting the production efficiency. Embodiment 2 uses a guide tube material with better heat insulation effect. The cooling rate of the crystal rod is fast, and the pulling rate of the crystal rod is increased to above the limit pulling speed of 0.65mm/min. Even if it reaches 0.7mm/min, the crystal rod does not break down. Distorted. Combining Example 1 and Example 2, it can be seen that by enhancing the heat insulation capability of the flow guide tube, the cooling rate of the crystal ingot is increased, which is beneficial to improving the problem of crystal ingot deformation at high pulling speeds.
實施例1和實施例3的晶棒熱歷史曲線如圖8所示，實施例1和實施例3的晶棒縱切缺陷分佈如圖9所示。實施例1中，由於晶棒冷却速率過快，導致最終獲得的晶棒徑向缺陷分佈差異過大，而無法生長出完整的完美晶體窗口（即晶棒中存在一橫截面，位於該橫截面處的晶體均為完美晶體）。實施例3中晶棒冷却速率適中，最終獲得的晶棒徑向缺陷分佈較為均勻，從而生長出完整的完美晶體窗口，進而形成完美晶圓。結合實施例3與實施例1可知，當晶棒內部缺陷分佈類似實施例1時，無法生長形成完美晶圓，透過增加導流筒與熔湯液面的距離，降低晶棒冷却速率，可以對缺陷分佈進行改善。The thermal history curves of the crystal ingots of Examples 1 and 3 are shown in Figure 8, and the longitudinal cutting defect distributions of the crystal ingots of Examples 1 and 3 are shown in Figure 9. In Example 1, because the cooling rate of the crystal rod is too fast, the radial defect distribution of the finally obtained crystal rod is too different, and a complete and perfect crystal window cannot be grown (that is, there is a cross-section in the crystal rod, located at the cross-section The crystals are all perfect crystals). In Example 3, the cooling rate of the crystal rod is moderate, and the radial defect distribution of the finally obtained crystal rod is relatively uniform, thereby growing a complete and perfect crystal window, thereby forming a perfect wafer. Combining Embodiment 3 and Embodiment 1, it can be seen that when the internal defect distribution of the crystal rod is similar to that of Embodiment 1, a perfect wafer cannot be grown. By increasing the distance between the guide tube and the molten liquid surface and reducing the cooling rate of the crystal rod, the wafer can be processed. Defect distribution is improved.
實施例4的晶棒熱歷史曲線如圖10所示，實施例4與實施例5的晶棒熱歷史曲線如圖11所示。實施例4中晶棒冷却速率較慢，作業時間較長，透過根據圖10中的晶棒熱歷史曲線進行調整後，結合實施例4與實施例5可知，吊料晶棒按照實施例5的冷却速率進行時無炸裂發生，且較實施例4節約1.45小時時間。也就是說實際生産中若存在晶棒炸裂情况，可採用本申請的方法首先得到炸裂測試曲線，進而有目的地調整晶棒熱歷史，只要調整後的晶棒冷却速率小於炸裂測試的冷却速率，就可以避免炸裂的發生，進而提高産品良率，提高生産效率。The thermal history curve of the crystal ingot of Example 4 is shown in Figure 10 , and the thermal history curves of the crystal ingot of Example 4 and Example 5 are shown in Figure 11 . In Example 4, the cooling rate of the crystal ingot is slower and the operation time is longer. After adjusting according to the thermal history curve of the crystal ingot in Figure 10, it can be seen from the combination of Example 4 and Example 5 that the crystal ingot is lifted according to the method of Example 5. No explosion occurred when the cooling rate was increased, and 1.45 hours was saved compared to Example 4. That is to say, if there is a crystal ingot burst in actual production, the method of this application can be used to first obtain the burst test curve, and then adjust the crystal ingot thermal history purposefully, as long as the adjusted cooling rate of the crystal ingot is less than the cooling rate of the burst test, This can avoid the occurrence of explosion, thereby improving product yield and production efficiency.
除非另外說明，本申請所使用的所有科技術語具有與所屬技術領域中具有通常知識者的通常理解相同的含義。本申請涉及的所有專利和公開出版物透過引用方式整體並入本申請。術語「包含」或「包括」為開放式表達，即包括本申請所指明的內容，但並不排除其他方面的內容。Unless otherwise stated, all technical and scientific terms used in this application have the same meanings as commonly understood by a person of ordinary skill in the art. All patents and publications referred to in this application are incorporated by reference in their entirety. The term "includes" or "includes" is an open expression, which includes the content specified in this application, but does not exclude other aspects.
在本申請的描述中，「A和/或B」可以包括單獨A的情况，單獨B的情况，A和B的情况的任一種，其中A、B僅用於舉例，其可以是本申請中使用「和/或」連接的任意技術特徵。In the description of this application, "A and/or B" may include the situation of A alone, the situation of B alone, or the situations of A and B, where A and B are only used as examples, which may be in this application. Any technical characteristics connected using "and/or".
在本說明書的描述中，參考術語「一個實施例」、「另一個實施例」等的描述意指結合該實施例描述的具體特徵、結構、材料或者特點包含於本申請的至少一個實施例中。在本說明書中，對上述術語的示意性表述不必須針對的是相同的實施例或示例。而且，描述的具體特徵、結構、材料或者特點可以在任一個或多個實施例或示例中以合適的方式結合。此外，在不相互矛盾的情况下，所屬技術領域中具有通常知識者可以將本說明書中描述的不同實施例或示例以及不同實施例或示例的特徵進行結合和組合。In the description of this specification, reference to the terms "one embodiment," "another embodiment," etc. means that a particular feature, structure, material, or characteristic described in connection with the embodiment is included in at least one embodiment of the present application. . In this specification, the schematic expressions of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the specific features, structures, materials or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, a person of ordinary skill in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples unless they are inconsistent with each other.
儘管上面已經示出和描述了本申請的實施例，可以理解的是，上述實施例是示例性的，不能理解為對本申請的限制，所屬技術領域中具有通常知識者在本申請的範圍內可以對上述實施例進行變化、修改、替換和變型。Although the embodiments of the present application have been shown and described above, it can be understood that the above-mentioned embodiments are illustrative and should not be construed as limitations of the present application. A person with ordinary skill in the art can understand the scope of the present application within the scope of the present application. Changes, modifications, substitutions and variations are made to the above embodiments.
10:主爐室 20:石英坩堝 30:導流筒 40:副室 T0、T1、T2、T3、T4、T5、T6、T7:紅外測溫裝置 T 0:初始溫度 t 0:初始時間點 T 1、T 2、T 3:待測溫橫截面的溫度 t 1、t 2、t 3:測得待測溫橫截面的溫度時的時間點 S1~S5:步驟 d 1、d 2、d 3、d 4、d 5:紅外測溫裝置的測溫點和熔湯液面之間的距離 10: Main furnace room 20: Quartz crucible 30: Guide tube 40: Auxiliary chamber T0, T1, T2, T3, T4, T5, T6, T7: Infrared temperature measurement device T 0 : Initial temperature t 0 : Initial time point T 1 , T 2 , T 3 : Temperature of the cross-section to be measured t 1 , t 2 , t 3 : Time points when the temperature of the cross-section to be measured is measured S1~S5: Steps d 1 , d 2 , d 3 , d 4 , d 5 : the distance between the temperature measurement point of the infrared temperature measurement device and the molten liquid level
本申請的上述和/或附加的方面和優點從結合下面附圖對實施例的描述中將變得明顯和容易理解，其中： 圖1顯示了根據本申請一個實施例單晶爐的結構示意圖； 圖2顯示了根據本申請又一個實施例單晶爐的結構示意圖； 圖3顯示了根據本申請一個實施例獲得晶棒熱歷史曲線的流程示意圖； 圖4顯示了根據本申請又一個實施例獲得晶棒熱歷史曲線的流程示意圖； 圖5顯示了根據本申請一個實施例的晶棒熱歷史曲線圖； 圖6顯示了實施例1中的晶棒熱歷史曲線圖； 圖7顯示了實施例1和實施例2中的晶棒熱歷史曲線圖； 圖8顯示了實施例1和實施例3中的晶棒熱歷史曲線圖； 圖9顯示了實施例1和實施例3中的晶棒縱切缺陷分佈； 圖10顯示了實施例4中的晶棒熱歷史曲線圖； 圖11顯示了實施例4和實施例5中的晶棒熱歷史曲線圖。 The above and/or additional aspects and advantages of the present application will become apparent and readily understood from the description of the embodiments in conjunction with the following drawings, in which: Figure 1 shows a schematic structural diagram of a single crystal furnace according to an embodiment of the present application; Figure 2 shows a schematic structural diagram of a single crystal furnace according to another embodiment of the present application; Figure 3 shows a schematic flow chart for obtaining the thermal history curve of a crystal ingot according to an embodiment of the present application; Figure 4 shows a schematic flow chart for obtaining the thermal history curve of a crystal ingot according to another embodiment of the present application; Figure 5 shows a thermal history curve of a crystal ingot according to an embodiment of the present application; Figure 6 shows the thermal history curve of the crystal rod in Example 1; Figure 7 shows the thermal history curves of the crystal ingots in Example 1 and Example 2; Figure 8 shows the thermal history curves of the crystal ingots in Example 1 and Example 3; Figure 9 shows the distribution of defects in the longitudinal cutting of the crystal rod in Example 1 and Example 3; Figure 10 shows the thermal history curve of the ingot in Example 4; Figure 11 shows the thermal history graphs of the ingots in Example 4 and Example 5.
S1~S4:步驟 S1~S4: steps
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