TWI732719B - Vacuum method for preventing dust explosion in production of phosphorus-doped monocrystalline silicon and production method of phosphorus-doped monocrystalline silicon using the same - Google Patents

Vacuum method for preventing dust explosion in production of phosphorus-doped monocrystalline silicon and production method of phosphorus-doped monocrystalline silicon using the same Download PDF

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TWI732719B
TWI732719B TW109142263A TW109142263A TWI732719B TW I732719 B TWI732719 B TW I732719B TW 109142263 A TW109142263 A TW 109142263A TW 109142263 A TW109142263 A TW 109142263A TW I732719 B TWI732719 B TW I732719B
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TW202126865A (en
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萬軍召
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大陸商鄭州合晶矽材料有限公司
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B35/00Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17DPIPE-LINE SYSTEMS; PIPE-LINES
    • F17D1/00Pipe-line systems
    • F17D1/02Pipe-line systems for gases or vapours
    • F17D1/04Pipe-line systems for gases or vapours for distribution of gas
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17DPIPE-LINE SYSTEMS; PIPE-LINES
    • F17D3/00Arrangements for supervising or controlling working operations
    • F17D3/01Arrangements for supervising or controlling working operations for controlling, signalling, or supervising the conveyance of a product
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

本發明公開了一種摻磷單晶矽生產中防塵爆的抽真空方法,用於生產摻磷單晶矽的單晶爐包括相互連通的主室和副室,所述副室設於所述主室上方;所述抽真空方法包括以下步驟:S1、採用第一管道將主閥和主泵依次連通到所述主室,並關閉所述主閥和主泵;S2、採用第二管道將輔助閥和副泵依次連通到所述副室,採用第三管道將快充閥連通至所述主室或所述副室;打開所述輔助閥和副泵將所述單晶爐內的空氣抽出,控制所述快充閥向所述單晶爐內通入惰性氣體。通過上述抽真空方法,可以實現逐漸減少爐內的空氣含量,在抽真空的同時不滿足塵爆條件;本發明中還提供了應用該防塵爆的抽真空方法的摻磷單晶矽生產方法,提供了安全生產摻磷單晶矽的保證。The invention discloses a vacuum method for preventing dust explosion in the production of phosphorus-doped single crystal silicon. A single crystal furnace used for the production of phosphorus-doped single crystal silicon includes a main chamber and a sub-chamber which are connected to each other, and the sub-chamber is arranged in the main Above the chamber; the vacuuming method includes the following steps: S1, using a first pipeline to connect the main valve and the main pump to the main chamber in turn, and closing the main valve and the main pump; S2, using a second pipeline to assist The valve and the auxiliary pump are sequentially connected to the auxiliary chamber, and a third pipe is used to connect the quick-fill valve to the main chamber or the auxiliary chamber; the auxiliary valve and the auxiliary pump are opened to extract the air in the single crystal furnace , Controlling the quick filling valve to pass inert gas into the single crystal furnace. Through the above-mentioned vacuuming method, the air content in the furnace can be gradually reduced, and the dust explosion conditions are not met while vacuuming; the present invention also provides a phosphorus-doped monocrystalline silicon production method using the dust-proof vacuuming method. Provides a guarantee for the safe production of phosphorus-doped monocrystalline silicon.

Description

摻磷單晶矽生產中防塵爆的抽真空方法及應用其的摻磷單晶矽生產方法Vacuum method for preventing dust explosion in production of phosphorus-doped monocrystalline silicon and production method of phosphorus-doped monocrystalline silicon using the same

本發明涉及半導體單晶矽的製造領域,尤其涉及一種摻磷單晶矽生產中防塵爆的抽真空方法及應用其的摻磷單晶矽生產方法。The invention relates to the manufacturing field of semiconductor single crystal silicon, in particular to a dust-proof vacuuming method in the production of phosphorus-doped single crystal silicon and a method for producing phosphorus-doped single crystal silicon using the same.

在半導體行業中,隨著積體電路技術的應用和發展,要求功率器件的功耗越來越低,尤其提出了電阻率更低的要求。在目前的研究中,相比於砷和銻,磷在矽晶格中的固溶度更大,得到的摻磷單晶矽的電阻率更低。目前用於生產單晶矽的單晶爐通常包括上下設置的副腔室和主腔室,用於放置原料多晶矽和紅磷的石英坩堝設於主腔室內;從連通到主腔室的管道抽真空時,副腔室和主腔室內的氣體通過上述管道經過打開的主閥和主泵被抽出。一旦開始生產單晶矽,該管道、主閥和主泵則24小時不間斷運行使單晶爐內保持真空狀態,這就導致了其使用的時間較長,在該管道內更容易沉積生產原料、磷和氧化物等物質。設置在主閥和主泵之間的管道由於設計等原因無法將其內的沉積物清理乾淨,雖然可以清洗主腔室、副腔室以及主腔室和主閥之間的管道內,但仍不可避免會有殘留物。當再次生產摻磷單晶矽打開主閥抽真空時,由於無法清洗乾淨的沉積物和殘留物中含有燃點低的紅磷,輕微摩擦如打開主閥產生的摩擦會導致紅磷氧化物粉塵爆炸的發生。一次塵爆將會污染高達130kg的高純度原料,甚至會使單晶爐內的石英坩堝、熱場部件和設備的損壞,不僅提高了生產維護成本,還給實際工作帶來了很大的危險。In the semiconductor industry, with the application and development of integrated circuit technology, the power consumption of power devices is required to be lower and lower, especially the requirement of lower resistivity. In the current study, compared with arsenic and antimony, phosphorus has a greater solid solubility in the silicon lattice, and the resulting phosphorus-doped single crystal silicon has a lower resistivity. The single crystal furnace currently used for the production of single crystal silicon usually includes a sub-chamber and a main chamber set up and down. The quartz crucible for placing the raw material polysilicon and red phosphorus is set in the main chamber; When vacuuming, the gas in the sub-chamber and the main chamber is pumped out through the open main valve and the main pump through the above-mentioned pipeline. Once the production of monocrystalline silicon is started, the pipeline, main valve and main pump will operate continuously for 24 hours to keep the vacuum in the monocrystalline furnace, which leads to a longer period of use, and it is easier to deposit production raw materials in the pipeline. , Phosphorus and oxides. The pipeline set between the main valve and the main pump cannot be cleaned of deposits due to design and other reasons. Although the main chamber, the sub-chamber, and the pipeline between the main chamber and the main valve can be cleaned, it is still There will inevitably be residues. When the phosphorous-doped monocrystalline silicon is reproduced and the main valve is opened for vacuuming, the deposits and residues that cannot be cleaned contain red phosphorous with a low ignition point, and slight friction such as the friction caused by opening the main valve will cause the red phosphorous oxide dust to explode. happened. A dust explosion will pollute up to 130kg of high-purity raw materials, and even damage the quartz crucible, thermal field components and equipment in the single crystal furnace, which not only increases the production and maintenance costs, but also brings great danger to the actual work. .

有鑑於此,吾等發明人乃潛心進一步研究,並著手進行研發及改良,期以一較佳發明以解決上述問題,且在經過不斷試驗及修改後而有本發明之問世。In view of this, our inventors devoted themselves to further research, and proceeded to develop and improve, hoping to develop a better invention to solve the above problems, and after continuous experimentation and modification, the present invention came out.

本發明為解決生產摻磷單晶矽的單晶爐內在開始生產單晶矽前抽真空時發生的塵爆問題,提供一種摻磷單晶矽生產中防塵爆的抽真空方法及應用其的摻磷單晶矽生產方法。In order to solve the dust explosion problem in the single crystal furnace for the production of phosphorus-doped monocrystalline silicon before the production of monocrystalline silicon is started, the invention provides a dust explosion-proof vacuum method in the production of phosphorus-doped monocrystalline silicon and its doping method. Phosphorus monocrystalline silicon production method.

為實現以上目的,根據本發明的一個方面,本發明通過以下技術方案實現:In order to achieve the above objectives, according to one aspect of the present invention, the present invention is achieved through the following technical solutions:

一種摻磷單晶矽生產中防塵爆的抽真空方法,用於生產摻磷單晶矽的單晶爐包括相互連通的主室和副室,所述副室設於所述主室上方;所述防塵爆的抽真空方法包括以下步驟:A vacuum method for preventing dust explosion in the production of phosphorus-doped single crystal silicon. A single crystal furnace used for the production of phosphorus-doped single crystal silicon includes a main chamber and an auxiliary chamber that are connected to each other, and the auxiliary chamber is arranged above the main chamber; The vacuum method for preventing dust explosion includes the following steps:

S1、採用第一管道將主閥和主泵依次連通到所述主室,並關閉所述主閥和主泵;S1. Use a first pipeline to connect the main valve and the main pump to the main chamber in sequence, and close the main valve and the main pump;

S2、採用第二管道將輔助閥和副泵依次連通到所述副室,採用第三管道將快充閥連通至所述主室或所述副室;打開所述輔助閥和副泵將所述單晶爐內的空氣抽出,控制所述快充閥向所述單晶爐內通入惰性氣體。S2. A second pipeline is used to connect the auxiliary valve and the auxiliary pump to the auxiliary chamber in sequence, and a third pipeline is used to connect the quick-fill valve to the main chamber or the auxiliary chamber; The air in the single crystal furnace is exhausted, and the quick filling valve is controlled to pass inert gas into the single crystal furnace.

優選地,步驟S2包括:Preferably, step S2 includes:

(1)設置惰性氣體流量;(1) Set the flow of inert gas;

(2)打開所述輔助閥和副泵將所述單晶爐內的空氣經所述第二管道抽出,爐壓降至P 1值時關閉所述輔助閥; (2) opening said auxiliary valve and said auxiliary pump crystal furnace through the second air extraction duct, the furnace pressure decreased to close the pilot valve P value of 1;

(3)打開所述快充閥且經所述第三管道向所述單晶爐內通入惰性氣體,爐壓升至P 2值時關閉所述快充閥。 (3) Open the fast charging valve and pass inert gas into the single crystal furnace through the third pipeline, and close the fast charging valve when the furnace pressure rises to the P 2 value.

優選地,依次重複步驟(2)和(3)操作至少三次後,爐壓為P 2值,同時所述輔助閥、副泵和快充閥保持關閉,再打開連通到主室上的主閥和主泵繼續抽出空氣保持單晶爐內真空狀態。 Preferably, after repeating steps (2) and (3) for at least three times, the furnace pressure is P 2 value, while the auxiliary valve, the auxiliary pump and the fast charging valve are kept closed, and then the main valve connected to the main chamber is opened Continue to pump out air with the main pump to maintain the vacuum state in the single crystal furnace.

優選地,打開主閥和主泵繼續抽出空氣前,還需要打開設置在所述主閥和主室之間的蝶閥,將所述蝶閥開度設為5%並打開所述蝶閥。Preferably, before opening the main valve and the main pump to continue to pump air, it is also necessary to open the butterfly valve provided between the main valve and the main chamber, set the butterfly valve opening to 5%, and open the butterfly valve.

優選地,惰性氣體包括氬氣,惰性氣體經所述第三管道從惰性氣體源送至所述快充閥。Preferably, the inert gas includes argon, and the inert gas is sent from the inert gas source to the fast filling valve through the third pipeline.

優選地,所述主室和副室之間設置有隔離閥來控制所述主室和副室的連通或隔離;在抽出空氣和通入惰性氣體的過程中,打開所述隔離閥以使所述主室和副室之間連通。Preferably, an isolation valve is provided between the main chamber and the auxiliary chamber to control the communication or isolation of the main chamber and the auxiliary chamber; in the process of extracting air and introducing inert gas, the isolation valve is opened to make the The main chamber and the auxiliary chamber are connected.

根據本發明的另一個方面,提供一種避免塵爆發生的摻磷單晶矽的生產方法。通過以下技術方案實現:According to another aspect of the present invention, there is provided a production method of phosphorus-doped single crystal silicon to avoid dust explosion. Realized through the following technical solutions:

一種避免塵爆發生的摻磷單晶矽的生產方法,包括以下步驟:A production method of phosphorus-doped monocrystalline silicon to avoid dust explosions, including the following steps:

將原料多晶矽加入單晶爐的主室內,通過上述的摻磷單晶矽生產中防塵爆的抽真空方法使爐內形成真空和通入惰性氣體,再加熱原料使其熔化後開始長晶進行摻磷單晶矽的生產。The raw material polycrystalline silicon is put into the main chamber of the single crystal furnace, and the dust-proof vacuum method in the production of phosphorus-doped single crystal silicon is used to form a vacuum in the furnace and inert gas is introduced, and then the raw material is heated to melt it, and then the crystal grows for mixing. Production of phosphorous monocrystalline silicon.

本發明中,“主室”為單晶爐中“主爐室”的簡稱;“副室”為單晶爐中“副爐室”的簡稱。In the present invention, the "main chamber" is the abbreviation of the "main furnace chamber" in the single crystal furnace; the "sub chamber" is the abbreviation of the "auxiliary furnace chamber" in the single crystal furnace.

本發明提供一種摻磷單晶矽生產中防塵爆的抽真空方法,在該方法中從單晶爐內的副室上連通的管道抽取出副室和主室的空氣,並從單晶爐的副室或主室上通入惰性氣體。由於連通到副室的第二管道的使用頻率較低,並且通過清洗可以將該管道內的附著物或沉積物清洗出,在抽出空氣時,少量的無法清理完全的殘留物也無法滿足塵爆的條件,而不會發生塵爆。而且,通過多次的抽取爐內空氣和向爐內通入惰性氣體的操作,可以實現逐漸減少爐內的空氣含量,同時不滿足塵爆條件,從而在打開主閥持續抽出空氣保持爐內真空狀態時不會發生塵爆問題。The invention provides a vacuum method for preventing dust explosion in the production of phosphorus-doped single crystal silicon. In the method, the air in the auxiliary chamber and the main chamber is extracted from the pipe connected to the auxiliary chamber in the single crystal furnace, and the air in the auxiliary chamber and the main chamber is extracted from the single crystal furnace. Inert gas is introduced into the auxiliary chamber or the main chamber. Since the second pipe connected to the auxiliary chamber is used less frequently, and the attachments or deposits in the pipe can be cleaned out by cleaning, when the air is pumped out, a small amount of residue that cannot be completely cleaned can not meet the dust explosion. Conditions without a dust explosion. Moreover, by repeatedly extracting the air in the furnace and introducing inert gas into the furnace, the air content in the furnace can be gradually reduced without meeting the conditions of dust explosion, so that the main valve is opened and the air is continuously drawn to maintain the vacuum in the furnace. No dust explosion problem occurs during the state.

本發明中還提供了應用該防塵爆的抽真空方法的摻磷單晶矽生產方法,由於該抽真空方法避免了塵爆的發生,也就有效地防止原料被污染、設備被破壞,無須花費時間去維修設備或回收原料。因此,本發明的生產方法提供了安全生產摻磷單晶矽的保證,避免塵爆的同時降低生產成本,避免了報廢原料的更換和維修設備的成本問題。The present invention also provides a method for producing phosphorous-doped monocrystalline silicon using the dust-proof vacuuming method. Because the vacuuming method avoids the occurrence of dust explosions, it also effectively prevents raw materials from being contaminated and equipment from being destroyed without cost. Time to repair equipment or recycle materials. Therefore, the production method of the present invention provides a guarantee for the safe production of phosphorus-doped monocrystalline silicon, reduces production costs while avoiding dust explosions, and avoids the cost problems of replacement of scrapped materials and maintenance of equipment.

關於吾等發明人之技術手段,茲舉數種較佳實施例配合圖式於下文進行詳細說明,俾供  鈞上深入了解並認同本發明。Regarding the technical means of our inventors, several preferred embodiments are described in detail below in conjunction with the drawings, in order to provide a thorough understanding and approval of the present invention.

下面結合實施例對本發明進行詳細的描述。The present invention will be described in detail below in conjunction with embodiments.

本發明提供的一種摻磷單晶矽生產中防塵爆的抽真空方法,用於生產摻磷單晶矽的單晶爐包括相互連通的主室和副室,其中副室設於主室上方;本發明的防塵爆的抽真空方法包括以下步驟:The invention provides a vacuum method for preventing dust explosion in the production of phosphorus-doped single crystal silicon. The single crystal furnace used for the production of phosphorus-doped single crystal silicon includes a main chamber and an auxiliary chamber that are connected to each other, wherein the auxiliary chamber is arranged above the main chamber; The vacuuming method for dust explosion prevention of the present invention includes the following steps:

S1、採用第一管道將主閥和主泵依次連通到主室,並關閉主閥和主泵;S1. Use the first pipeline to connect the main valve and the main pump to the main chamber in turn, and close the main valve and the main pump;

S2、採用第二管道將輔助閥和副泵依次連通到副室,採用第三管道將快充閥連通至主室或副室;打開輔助閥和副泵將單晶爐內的空氣抽出,並控制快充閥向單晶爐內通入惰性氣體。S2. Use the second pipeline to connect the auxiliary valve and the auxiliary pump to the auxiliary chamber in turn, and use the third pipeline to connect the quick-fill valve to the main chamber or the auxiliary chamber; open the auxiliary valve and the auxiliary pump to extract the air in the single crystal furnace, and Control the quick filling valve to pass inert gas into the single crystal furnace.

通過連通到副室上的第二管道和輔助閥將空氣從副室和主室中逐漸抽出,以減少單晶爐內的含氧量,並向單晶爐內通入惰性氣體;通過該抽真空方法使單晶爐內形成真空並在惰性氣體保護下開始熔化多晶矽原料生長單晶矽。在本發明的抽真空方法中顯著減少紅磷氧化物發生粉塵爆炸;有效避免了主室、副室或者第一管道、第二管道中紅磷的附著物或沉積物導致的爆炸問題。The air is gradually extracted from the auxiliary chamber and the main chamber through the second pipe and auxiliary valve connected to the auxiliary chamber to reduce the oxygen content in the single crystal furnace, and inert gas is introduced into the single crystal furnace; The vacuum method creates a vacuum in the single crystal furnace and starts to melt the polycrystalline silicon raw material to grow single crystal silicon under the protection of inert gas. In the vacuuming method of the present invention, the dust explosion of red phosphorus oxide is significantly reduced; the explosion problem caused by red phosphorus attachments or deposits in the main chamber, the auxiliary chamber, or the first pipe and the second pipe is effectively avoided.

上述步驟S2包括:The above step S2 includes:

(1)設置惰性氣體流量;(1) Set the flow of inert gas;

(2)打開輔助閥和副泵將所述單晶爐內的空氣經第二管道抽出,爐壓降至P 1值時關閉輔助閥; (2) opens the auxiliary valve and said auxiliary pump through the second single-crystal furnace air extraction duct, the furnace pressure decreased to close the secondary valve when the value of P 1;

(3)打開快充閥且經第三管道向單晶爐內通入惰性氣體,爐壓升至P 2值時關閉快充閥。 (3) Open the fast-fill valve and pass inert gas into the single crystal furnace through the third pipe, and close the fast-fill valve when the furnace pressure rises to the P 2 value.

在摻磷單晶矽生產的抽真空時,可根據實際單晶爐的狀況和所要生產的單晶矽等因素適當調節步驟(2)和(3)的爐壓P 1值和P 2值,並且P 2值大於P 1值。 When vacuuming the production of phosphorous-doped single crystal silicon, the furnace pressure P 1 value and P 2 value of steps (2) and (3) can be adjusted appropriately according to the actual single crystal furnace conditions and the single crystal silicon to be produced. And the value of P 2 is greater than the value of P 1 .

依次重複步驟(2)和(3)操作至少三次後,爐壓為P 2值,同時輔助閥、副泵和快充閥保持關閉,再打開連通到主室上的主閥和主泵繼續抽出空氣保持單晶爐內真空狀態。 After repeating steps (2) and (3) for at least three times, the furnace pressure is P 2 value, while the auxiliary valve, auxiliary pump and fast charging valve are kept closed, and then the main valve and main pump connected to the main chamber are opened to continue pumping The air maintains the vacuum state in the single crystal furnace.

在生產摻磷單晶矽的過程中,連通到副室的第二管道使用頻率較低,並且通過清洗可以將管道內的附著物或沉積物清洗出,通過第二管道抽取氣體時,少量的無法清理完全的殘留物也無法滿足塵爆的條件而不會發生塵爆。In the process of producing phosphorous-doped monocrystalline silicon, the second pipeline connected to the auxiliary chamber is used less frequently, and the attachments or deposits in the pipeline can be cleaned out by cleaning. When gas is extracted through the second pipeline, a small amount of Residues that cannot be completely cleaned up cannot meet the conditions of a dust explosion without a dust explosion.

打開輔助閥抽出空氣後,打開連通至單晶爐的主室或是副室的快充閥,向單晶爐內通入惰性氣體,快速置換爐內空氣。該快充閥也可以連通至單晶爐的主室和副室之間的相連通處,從主室和副室相連通的地方通入惰性氣體。通過控制該快充閥,惰性氣體逐漸從連接至惰性氣體源的第三管道通入主室和副室內。After opening the auxiliary valve to extract air, open the fast filling valve connected to the main chamber or the auxiliary chamber of the single crystal furnace, and pass inert gas into the single crystal furnace to quickly replace the air in the furnace. The fast filling valve can also be connected to the communication between the main chamber and the auxiliary chamber of the single crystal furnace, and inert gas is introduced from the communication place between the main chamber and the auxiliary chamber. By controlling the fast filling valve, the inert gas gradually flows into the main chamber and the sub-chamber from the third pipe connected to the inert gas source.

打開主閥和主泵繼續抽出空氣前,還需要打開設置在所述主閥和主室之間的蝶閥,將所述蝶閥開度設為5%後打開該蝶閥。然後才打開主閥和主泵繼續抽真空使主室和副室在開始加熱生產單晶矽前形成真空,並在生產單晶矽後持續保持真空狀態。此時,雖然主泵和主閥之間管路內的附著物無法清洗出,但由於單晶爐內已處於含氧量較低的真空狀態,而無法滿足塵爆的條件、避免了塵爆的發生。並且,蝶閥是在生產單晶矽過程中主要起到自動調節爐壓的作用,此時先將蝶閥開度設為5%,則是為了防止氣流摩擦過大,進一步防止塵爆。Before opening the main valve and the main pump to continue to pump air, the butterfly valve provided between the main valve and the main chamber also needs to be opened, and the butterfly valve is opened after setting the opening degree of the butterfly valve to 5%. Then, the main valve and the main pump are opened to continue vacuuming, so that the main chamber and the sub-chamber form a vacuum before heating to produce monocrystalline silicon, and continue to maintain a vacuum state after monocrystalline silicon is produced. At this time, although the attachments in the pipeline between the main pump and the main valve cannot be cleaned out, the single crystal furnace is already in a vacuum with low oxygen content, which cannot meet the conditions of dust explosion and avoid dust explosion. happened. In addition, the butterfly valve is mainly used to automatically adjust the furnace pressure during the production of monocrystalline silicon. At this time, the butterfly valve opening is set to 5% to prevent excessive air friction and further prevent dust explosion.

惰性氣體包括氬氣,惰性氣體經第三管道從惰性氣體源送至快充閥。The inert gas includes argon, and the inert gas is sent from the inert gas source to the fast filling valve through the third pipeline.

主泵採用水泵。The main pump is a water pump.

主室和副室之間設置有隔離閥來控制主室和副室的連通或隔離;在抽出空氣和通入惰性氣體的過程中,打開隔離閥以使主室和副室之間連通。An isolation valve is arranged between the main chamber and the auxiliary chamber to control the communication or isolation between the main chamber and the auxiliary chamber; in the process of extracting air and introducing inert gas, the isolation valve is opened to communicate between the main chamber and the auxiliary chamber.

本發明還提供了一種避免塵爆發生的摻磷單晶矽的生產方法,包括以下步驟:The present invention also provides a production method of phosphorus-doped monocrystalline silicon to avoid dust explosion, which includes the following steps:

將原料多晶矽加入單晶爐的主室內,通過上述的摻磷單晶矽生產中防塵爆的抽真空方法使爐內形成真空和通入惰性氣體,再加熱原料使其熔化後開始長晶進行摻磷單晶矽的生產。The raw material polycrystalline silicon is put into the main chamber of the single crystal furnace, and the dust-proof vacuum method in the production of phosphorus-doped single crystal silicon is used to form a vacuum in the furnace and inert gas is introduced, and then the raw material is heated to melt it, and then the crystal grows for mixing. Production of phosphorous monocrystalline silicon.

實施例1Example 1

用於生產摻磷單晶矽的單晶爐包括相連通的主室和副室,並且副室設置在主室上方,副室和主室之間設置有隔離閥控制二者之間的連通或隔離;通過第一管道依次將主閥、主泵連通到主室,通過第二管道依次將輔助閥、副泵連通至副室,通過第三管道將惰性氣體源和快充閥依次連通至主室。將原料多晶矽放入主室內的石英坩堝內,開始準備抽單晶爐內的空氣。The single crystal furnace used to produce phosphorous-doped single crystal silicon includes a main chamber and a sub-chamber that are connected, and the sub-chamber is arranged above the main chamber. An isolation valve is set between the sub-chamber and the main chamber to control the communication or Isolation; the main valve and the main pump are connected to the main chamber through the first pipeline, the auxiliary valve and the auxiliary pump are connected to the auxiliary chamber through the second pipeline, and the inert gas source and the fast filling valve are connected to the main chamber through the third pipeline. room. Put the raw material polysilicon into the quartz crucible in the main chamber, and start preparing to pump the air in the single crystal furnace.

打開設置在主室和副室之間的隔離閥,使主室和副室保持連通狀態。通過連通到單晶爐的充氣閥先向單晶爐內充入少量氬氣,打開單晶爐上的防爆閥乾粉排氣,進行爐內水分置換,然後關閉氬氣和防爆閥。關閉主閥和主泵,打開輔助閥和副泵,經第二管道從副室開始抽出空氣,在副泵的作用下將副室和主室內的空氣逐漸抽出。同時,打開快充閥,向單晶爐的副室和主室逐漸通入氬氣。根據單晶爐狀況及相應的生產情況,設定氬氣流量值、抽出空氣後的爐壓、通入惰性氣體後的爐壓以及單晶爐內真空等;本實施例中設定氬氣流量為50slpm,打開輔助閥、使用副泵來抽取爐內的空氣,使爐內壓力降至200Torr時關閉輔助閥和副泵;打開快充閥向單晶爐內通入氬氣,並使爐內壓力升至400Torr時關閉快充閥。再次,打開輔助閥和副泵抽取空氣使爐內壓力降至200Torr後將其關閉;打開快充閥通氬氣使爐內壓力升至400Torr後將其關閉,並繼續重複一次上述兩步操作。完成三次空氣抽出和通入氬氣的重複迴圈操作以使爐壓穩定至400Torr後,關閉輔助閥和副泵。打開主閥和主泵,並將設置在主閥和主室之間的蝶閥的開度設置為5%,繼續完成抽真空使單晶爐內形成並保持真空狀態。The isolation valve provided between the main chamber and the auxiliary chamber is opened to keep the main chamber and the auxiliary chamber in communication. A small amount of argon is filled into the single crystal furnace through the charging valve connected to the single crystal furnace, the explosion-proof valve on the single crystal furnace is opened to exhaust the dry powder, the moisture in the furnace is replaced, and then the argon gas and the explosion-proof valve are closed. Close the main valve and the main pump, open the auxiliary valve and the auxiliary pump, and start to extract air from the auxiliary chamber through the second pipe, and gradually extract the air in the auxiliary chamber and the main chamber under the action of the auxiliary pump. At the same time, open the fast filling valve, and gradually introduce argon into the sub-chamber and main chamber of the single crystal furnace. According to the condition of the single crystal furnace and the corresponding production situation, set the argon flow value, the furnace pressure after the air is extracted, the furnace pressure after the inert gas is introduced, and the vacuum in the single crystal furnace; in this embodiment, the argon flow is set to 50 slpm , Open the auxiliary valve, use the auxiliary pump to extract the air in the furnace, close the auxiliary valve and the auxiliary pump when the pressure in the furnace drops to 200 Torr; open the fast filling valve to pass argon into the single crystal furnace, and increase the pressure in the furnace Close the fast-fill valve when it reaches 400 Torr. Once again, open the auxiliary valve and auxiliary pump to extract air to reduce the pressure in the furnace to 200 Torr and then close it; open the fast filling valve and ventilate argon to increase the pressure in the furnace to 400 Torr and then close it, and continue to repeat the above two steps. After completing three repeated loops of air extraction and argon introduction to stabilize the furnace pressure to 400 Torr, close the auxiliary valve and the auxiliary pump. Open the main valve and the main pump, and set the opening degree of the butterfly valve between the main valve and the main chamber to 5%, and continue to complete the vacuuming to form and maintain a vacuum state in the single crystal furnace.

完成抽真空後,開始加熱、熔化原料形成矽熔體,先關閉隔離閥使主室和副室變為隔離狀態,將氣相狀態的紅磷摻雜到主室內的矽熔體中,將籽晶插入矽熔體表面進行熔接,並依次進行引晶、放肩、轉肩、等徑生長及收尾後即得摻磷單晶矽。在上述過程中,避免了塵爆的發生,能夠順利運行繼續生產單晶。After the vacuum is completed, start to heat and melt the raw materials to form a silicon melt, first close the isolation valve to make the main chamber and the auxiliary chamber into an isolated state, dope the red phosphorus in the gas phase into the silicon melt in the main chamber, and remove the seed The crystal is inserted into the surface of the silicon melt for welding, followed by seeding, shoulder setting, shoulder turning, equal diameter growth and finishing to obtain phosphorus-doped single crystal silicon. In the above process, the occurrence of dust explosion is avoided, and the single crystal production can be continued smoothly.

實施例2Example 2

用於生產摻磷單晶矽的單晶爐的設置同實施例1。將原料多晶矽放入主室內的石英坩堝內,開始準備抽單晶爐內的空氣。打開隔離閥,使主室和副室保持連通狀態。通過連通到單晶爐的充氣閥先向單晶爐內充入少量氬氣,打開單晶爐上的防爆閥乾粉排氣,進行爐內水分置換,然後關閉氬氣和防爆閥。關閉主閥和主泵,打開輔助閥和副泵,經第二管道從副室開始抽出空氣,在副泵的作用下將副室和主室內的空氣逐漸抽出。同時,打開快充閥,向單晶爐的副室和主室逐漸通入氬氣。根據單晶爐狀況及相應的生產情況,設定氬氣流量值、抽出空氣後的爐壓、通入惰性氣體後的爐壓以及單晶爐內真空等;本實施例中設定氬氣流量為60slpm,打開輔助閥、使用副泵來抽取爐內的空氣,使爐內壓力降至300Torr時關閉輔助閥和副泵;打開快充閥向單晶爐內通入氬氣,並使爐內壓力升至600Torr時關閉快充閥。再次,打開輔助閥和副泵抽取空氣使爐內壓力降至300Torr後將其關閉;打開快充閥通氬氣使爐內壓力升至600Torr後將其關閉,並繼續重複上述兩步操作兩次。完成四次空氣抽出和通入氬氣的重複迴圈操作以使爐壓穩定至600Torr後,關閉輔助閥和副泵。打開主閥和主泵,並將設置在主閥和主室之間的蝶閥的開度設置為5%,繼續完成抽真空使單晶爐內形成並保持真空狀態。The setup of the single crystal furnace for producing phosphorous-doped single crystal silicon is the same as that of Example 1. Put the raw material polysilicon into the quartz crucible in the main chamber, and start preparing to pump the air in the single crystal furnace. Open the isolation valve to keep the main chamber and the auxiliary chamber in communication. A small amount of argon is filled into the single crystal furnace through the charging valve connected to the single crystal furnace, the explosion-proof valve on the single crystal furnace is opened to exhaust the dry powder, the moisture in the furnace is replaced, and then the argon gas and the explosion-proof valve are closed. Close the main valve and the main pump, open the auxiliary valve and the auxiliary pump, and start to extract air from the auxiliary chamber through the second pipe, and gradually extract the air in the auxiliary chamber and the main chamber under the action of the auxiliary pump. At the same time, open the fast filling valve, and gradually introduce argon into the sub-chamber and main chamber of the single crystal furnace. According to the conditions of the single crystal furnace and the corresponding production situation, set the argon flow value, the furnace pressure after the air is extracted, the furnace pressure after the inert gas is introduced, and the vacuum in the single crystal furnace; in this embodiment, the argon flow is set to 60 slpm , Open the auxiliary valve, use the auxiliary pump to extract the air in the furnace, close the auxiliary valve and the auxiliary pump when the pressure in the furnace drops to 300 Torr; open the fast filling valve to pass argon into the single crystal furnace and increase the pressure in the furnace Close the fast-fill valve when it reaches 600 Torr. Once again, open the auxiliary valve and the auxiliary pump to extract air to reduce the pressure in the furnace to 300 Torr and then close it; open the fast filling valve and ventilate argon to increase the pressure in the furnace to 600 Torr and then close it, and continue to repeat the above two steps twice. . After completing four repeated loop operations of air extraction and argon gas introduction to stabilize the furnace pressure to 600 Torr, close the auxiliary valve and the auxiliary pump. Open the main valve and the main pump, and set the opening degree of the butterfly valve between the main valve and the main chamber to 5%, and continue to complete the vacuuming to form and maintain a vacuum state in the single crystal furnace.

完成抽真空後,開始加熱、熔化原料形成矽熔體,先關閉隔離閥使主室和副室變為隔離狀態,將氣相狀態的紅磷摻雜到主室內的矽熔體中,將籽晶插入矽熔體表面進行熔接,並依次進行引晶、放肩、轉肩、等徑生長及收尾後即得摻磷單晶矽。After the vacuum is completed, start to heat and melt the raw materials to form a silicon melt, first close the isolation valve to make the main chamber and the auxiliary chamber into an isolated state, dope the red phosphorus in the gas phase into the silicon melt in the main chamber, and remove the seed The crystal is inserted into the surface of the silicon melt for welding, followed by seeding, shoulder setting, shoulder turning, equal diameter growth and finishing to obtain phosphorus-doped single crystal silicon.

實施例3Example 3

用於生產摻磷單晶矽的單晶爐的設置同實施例1。將原料多晶矽放入主室內的石英坩堝內,開始準備抽單晶爐內的空氣。打開隔離閥,使主室和副室保持連通狀態。通過連通到單晶爐的充氣閥先向單晶爐內充入少量氬氣,打開單晶爐上的防爆閥乾粉排氣,進行爐內水分置換,然後關閉氬氣和防爆閥。關閉主閥和主泵,打開輔助閥和副泵,經第二管道從副室開始抽出空氣,在副泵的作用下將副室和主室內的空氣逐漸抽出。同時,打開快充閥,向單晶爐的副室和主室逐漸通入氬氣。根據單晶爐狀況及相應的生產情況,設定氬氣流量值、抽出空氣後的爐壓、通入惰性氣體後的爐壓以及單晶爐內真空等;本實施例中設定氬氣流量為55slpm,打開輔助閥、使用副泵來抽取爐內的空氣,使爐內壓力降至250Torr時關閉輔助閥和副泵;打開快充閥向單晶爐內通入氬氣,並使爐內壓力升至550Torr時關閉快充閥。再次,打開輔助閥和副泵抽取空氣使爐內壓力降至250Torr後將其關閉;打開快充閥通氬氣使爐內壓力升至550Torr後將其關閉,並繼續重複上述兩步操作兩次。完成四次空氣抽出和通入氬氣的重複迴圈操作以使爐壓穩定至550Torr後,關閉輔助閥和副泵。打開主閥和主泵,並將設置在主閥和主室之間的蝶閥的開度設置為5%,繼續完成抽真空使單晶爐內形成並保持真空狀態。The setup of the single crystal furnace for producing phosphorous-doped single crystal silicon is the same as that of the first embodiment. Put the raw material polysilicon into the quartz crucible in the main chamber, and start preparing to pump the air in the single crystal furnace. Open the isolation valve to keep the main chamber and the auxiliary chamber in communication. A small amount of argon is filled into the single crystal furnace through the charging valve connected to the single crystal furnace, the explosion-proof valve on the single crystal furnace is opened to exhaust the dry powder, the moisture in the furnace is replaced, and then the argon gas and the explosion-proof valve are closed. Close the main valve and the main pump, open the auxiliary valve and the auxiliary pump, and start to extract air from the auxiliary chamber through the second pipe, and gradually extract the air in the auxiliary chamber and the main chamber under the action of the auxiliary pump. At the same time, open the fast filling valve, and gradually introduce argon into the sub-chamber and main chamber of the single crystal furnace. According to the conditions of the single crystal furnace and the corresponding production conditions, set the argon flow value, the furnace pressure after the air is extracted, the furnace pressure after the inert gas is introduced, and the vacuum in the single crystal furnace; in this embodiment, the argon flow is set to 55 slpm , Open the auxiliary valve, use the auxiliary pump to extract the air in the furnace, close the auxiliary valve and the auxiliary pump when the pressure in the furnace drops to 250 Torr; open the fast filling valve to pass argon into the single crystal furnace, and increase the pressure in the furnace Close the fast-fill valve when it reaches 550 Torr. Once again, open the auxiliary valve and the auxiliary pump to extract air to reduce the pressure in the furnace to 250 Torr and then close it; open the fast filling valve and ventilate argon to increase the pressure in the furnace to 550 Torr and then close it, and continue to repeat the above two steps twice. . After completing four repeated loops of air extraction and argon introduction to stabilize the furnace pressure to 550 Torr, close the auxiliary valve and the auxiliary pump. Open the main valve and the main pump, and set the opening degree of the butterfly valve between the main valve and the main chamber to 5%, and continue to complete the vacuum to form and maintain a vacuum state in the single crystal furnace.

完成抽真空後,開始加熱、熔化原料形成矽熔體,先關閉隔離閥使主室和副室變為隔離狀態,將氣相狀態的紅磷摻雜到主室內的矽熔體中,將籽晶插入矽熔體表面進行熔接,並依次進行引晶、放肩、轉肩、等徑生長及收尾後即得摻磷單晶矽。After the vacuum is completed, start to heat and melt the raw materials to form a silicon melt, first close the isolation valve to make the main chamber and the auxiliary chamber into an isolated state, dope the red phosphorus in the gas phase into the silicon melt in the main chamber, and remove the seed The crystal is inserted into the surface of the silicon melt for welding, followed by seeding, shoulder setting, shoulder turning, equal diameter growth and finishing to obtain phosphorus-doped single crystal silicon.

對比例1Comparative example 1

將原料多晶矽加入單晶爐主室內的石英坩堝中,打開設置在主室和副室之間的隔離閥,使主室和副室保持連通狀態。通過管道依次將主球閥、主泵連通到主室,其中主泵採用水泵,打開主閥,通過主泵的作用將單晶爐內的空氣抽出。在單晶爐的主室上通過管道連通有快充閥,通過快充閥的打開向單晶爐內通入氬氣。完成抽真空後,開始加熱、熔化原料形成矽熔體,先關閉隔離閥使主室和副室變為隔離狀態,將氣相狀態的紅磷摻雜到主室內的矽熔體中,將籽晶插入矽熔體表面進行熔接進行長晶。The raw material polycrystalline silicon is added to the quartz crucible in the main chamber of the single crystal furnace, and the isolation valve arranged between the main chamber and the auxiliary chamber is opened to keep the main chamber and the auxiliary chamber in a connected state. The main ball valve and the main pump are connected to the main chamber through pipelines. The main pump adopts a water pump. The main valve is opened and the air in the single crystal furnace is drawn out through the action of the main pump. A fast filling valve is connected to the main chamber of the single crystal furnace through a pipeline, and argon gas is introduced into the single crystal furnace through the opening of the fast filling valve. After the vacuum is completed, start to heat and melt the raw materials to form a silicon melt, first close the isolation valve to make the main chamber and the auxiliary chamber into an isolated state, dope the red phosphorus in the gas phase into the silicon melt in the main chamber, and remove the seed The crystal is inserted into the surface of the silicon melt for welding to grow crystals.

採用上述實施例1~3和對比例1中的方法均是通過運行一台單晶爐進行摻磷單晶矽的生產並且應用本發明的抽真空方法,得到的對比結果如表一所示。在進行上述生產時,對應測試時間內的生產次數,即表示一台單晶爐在該時間內完成同樣原料量生產摻磷單晶矽的次數,也代表了該單台單晶爐在該時間內抽真空的次數,並且每次生產前都會打開單晶爐進行清洗。The methods in the above-mentioned Examples 1 to 3 and Comparative Example 1 are all produced by operating a single crystal furnace to produce phosphorus-doped single crystal silicon and applying the vacuuming method of the present invention. The comparison results obtained are shown in Table 1. During the above-mentioned production, the number of productions corresponding to the test time indicates the number of times that a single crystal furnace has completed the same amount of raw material to produce phosphorus-doped single crystal silicon within that time, and it also represents the number of times that the single crystal furnace has been in this time. The number of times of vacuuming inside, and the single crystal furnace is opened for cleaning before each production.

[表一] 實施專案 測試時間 對應測試時間內的生產次數 塵爆次數 實施例1 6個月 15次 0 實施例2 12個月 28次 0 實施例3 6個月 15次 0 對比例1 6個月 9次 6次 [Table I] Implementation of the project testing time Corresponding to the number of productions within the test time Number of dust bursts Example 1 6 months 15 times 0 Example 2 12 months 28 times 0 Example 3 6 months 15 times 0 Comparative example 1 6 months 9 times 6 times

從對比例1和實施例1的對比上可以看出,同樣都在6個月的時間內,傳統方法不但會導致塵爆的發生,而且塵爆的發生會引起原料被污染、設備被破壞,需要更多時間去維修設備、回收原料,從而同樣時間內的生產次數也隨之降低,不僅需要花費更多時間還提高了成本。因此,從上述實施例1~3和對比例1的對比結果中可看出,採用本發明的防塵爆抽真空方法在生產摻磷單晶矽的過程中,均未發生塵爆問題,說明本發明中防塵爆的抽真空方法能夠保證每次生產不會發生塵爆。這也就使得應用該防塵爆的抽真空方法的摻磷單晶矽生產方法,在保證生產安全的同時,也避免了原料和設備部件的報廢和損壞,有利於降低生產成本。From the comparison between Comparative Example 1 and Example 1, it can be seen that the traditional methods will not only cause dust explosions, but also cause raw materials to be contaminated and equipment destroyed. It takes more time to repair equipment and recycle raw materials, so the number of productions in the same time is also reduced, which not only takes more time but also increases costs. Therefore, it can be seen from the comparison results of the foregoing Examples 1 to 3 and Comparative Example 1 that the dust explosion-proof vacuum method of the present invention does not cause dust explosion problems during the production of phosphorus-doped single crystal silicon. The vacuum method for preventing dust explosion in the invention can ensure that no dust explosion occurs in each production. This also enables the phosphorus-doped monocrystalline silicon production method using the dust-proof vacuum method to ensure production safety while avoiding the scrap and damage of raw materials and equipment parts, which is beneficial to reducing production costs.

本發明中的實施例僅用於對本發明進行說明,並不構成對申請專利範圍的限制,本發明所屬技術領域中具有通常知識者可以想到的其他實質上等同的替代,均在本發明保護範圍內。The embodiments of the present invention are only used to illustrate the present invention, and do not constitute a limitation on the scope of the patent application. Other substantially equivalent alternatives that can be thought of by those with ordinary knowledge in the technical field to which the present invention belongs are all within the protection scope of the present invention. Inside.

綜上所述,本發明所揭露之技術手段確能有效解決習知等問題,並達致預期之目的與功效,且申請前未見諸於刊物、未曾公開使用且具長遠進步性,誠屬專利法所稱之發明無誤,爰依法提出申請,懇祈  鈞上惠予詳審並賜准發明專利,至感德馨。In summary, the technical means disclosed in the present invention can effectively solve the conventional problems and achieve the expected purpose and effect. It has not been seen in the publications, has not been used publicly, and has long-term progress before the application. The patent law claims that the invention is correct. Yan filed an application in accordance with the law and prayed that Jun Shanghui would give a detailed examination and grant a patent for invention.

惟以上所述者,僅為本發明之數種較佳實施例,當不能以此限定本發明實施之範圍,即大凡依本發明申請專利範圍及發明說明書內容所作之等效變化與修飾,皆應仍屬本發明專利涵蓋之範圍內。However, the above are only a few preferred embodiments of the present invention, and should not be used to limit the scope of implementation of the present invention, that is, all equivalent changes and modifications made in accordance with the scope of the patent application of the present invention and the content of the description of the invention are all It should still fall within the scope of the patent for this invention.

no

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Claims (7)

一種摻磷單晶矽生產中防塵爆的抽真空方法,其特徵在於,用於生產摻磷單晶矽的單晶爐包括相互連通的主室和副室,所述副室設於所述主室上方;所述防塵爆的抽真空方法包括以下步驟: S1、採用第一管道將主閥和主泵依次連通到所述主室,並關閉所述主閥和主泵; S2、採用第二管道將輔助閥和副泵依次連通到所述副室,採用第三管道將快充閥連通至所述主室或所述副室;打開所述輔助閥和副泵將所述單晶爐內的空氣抽出,控制所述快充閥向所述單晶爐內通入惰性氣體。 A vacuum method for preventing dust explosion in the production of phosphorus-doped single crystal silicon, characterized in that, a single crystal furnace for producing phosphorus-doped single crystal silicon includes a main chamber and a sub-chamber communicating with each other, and the sub-chamber is arranged in the main Above the chamber; the vacuum method for preventing dust explosion includes the following steps: S1. Use a first pipeline to connect the main valve and the main pump to the main chamber in sequence, and close the main valve and the main pump; S2. A second pipeline is used to connect the auxiliary valve and the auxiliary pump to the auxiliary chamber in sequence, and a third pipeline is used to connect the quick-fill valve to the main chamber or the auxiliary chamber; The air in the single crystal furnace is exhausted, and the quick filling valve is controlled to pass inert gas into the single crystal furnace. 如請求項1所述之摻磷單晶矽生產中防塵爆的抽真空方法,其特徵在於,步驟S2包括: (1)設置惰性氣體流量; (2)打開所述輔助閥和副泵將所述單晶爐內的空氣經所述第二管道抽出,爐壓降至P 1值時關閉所述輔助閥; (3)打開所述快充閥且經所述第三管道向所述單晶爐內通入惰性氣體,爐壓升至P 2值時關閉所述快充閥。 The vacuum method for preventing dust explosion in the production of phosphorus-doped monocrystalline silicon as described in claim 1, characterized in that step S2 includes: (1) setting the flow of inert gas; (2) opening the auxiliary valve and the auxiliary pump The air in the single crystal furnace is drawn out through the second pipe, and the auxiliary valve is closed when the furnace pressure drops to the value of P 1 ; (3) The fast charging valve is opened and the single crystal is directed to the single crystal through the third pipe. Inert gas is introduced into the furnace, and the quick-fill valve is closed when the furnace pressure rises to the P 2 value. 如請求項2所述之摻磷單晶矽生產中防塵爆的抽真空方法,其中,依次重複步驟(2)和(3)操作至少三次後,爐壓為P 2值,同時所述輔助閥、副泵和快充閥保持關閉,再打開連通到主室上的主閥和主泵繼續抽出空氣保持單晶爐內真空狀態。 The vacuum method for preventing dust explosion in the production of phosphorus-doped monocrystalline silicon as described in claim 2, wherein, after steps (2) and (3) are repeated in sequence for at least three times, the furnace pressure is P 2 value, and the auxiliary valve , The auxiliary pump and the fast filling valve are kept closed, and then the main valve and the main pump connected to the main chamber are opened to continue to pump out air to maintain the vacuum state in the single crystal furnace. 如請求項3所述之摻磷單晶矽生產中防塵爆的抽真空方法,其中,打開主閥和主泵繼續抽出空氣前,還需要打開設置在所述主閥和主室之間的蝶閥,將所述蝶閥開度設為5%並打開所述蝶閥。The vacuum method for preventing dust explosion in the production of phosphorus-doped monocrystalline silicon as described in claim 3, wherein, before opening the main valve and the main pump to continue to pump out air, the butterfly valve provided between the main valve and the main chamber also needs to be opened , Set the butterfly valve opening to 5% and open the butterfly valve. 如請求項1至3項中任一項所述之摻磷單晶矽生產中防塵爆的抽真空方法,其中,惰性氣體包括氬氣,惰性氣體經所述第三管道從惰性氣體源送至所述快充閥。The vacuum method for preventing dust explosion in the production of phosphorus-doped single crystal silicon according to any one of claims 1 to 3, wherein the inert gas includes argon, and the inert gas is sent from the inert gas source to the The fast filling valve. 如請求項1至4項中任一項所述之摻磷單晶矽生產中防塵爆的抽真空方法,其中,所述主室和副室之間設置有隔離閥來控制所述主室和副室的連通或隔離;在抽出空氣和通入惰性氣體的過程中,打開所述隔離閥以使所述主室和副室之間連通。The vacuum method for preventing dust explosion in the production of phosphorus-doped single crystal silicon according to any one of claims 1 to 4, wherein an isolation valve is provided between the main chamber and the auxiliary chamber to control the main chamber and The communication or isolation of the auxiliary chamber; in the process of extracting air and introducing inert gas, the isolation valve is opened to make the communication between the main chamber and the auxiliary chamber. 一種避免塵爆發生的摻磷單晶矽的生產方法,其特徵在於,包括以下步驟: 將原料多晶矽加入單晶爐的主室內,通過如請求項1至6項中任一項所述之摻磷單晶矽生產中防塵爆的抽真空方法使爐內形成真空和通入惰性氣體,再加熱原料使其熔化後開始長晶進行摻磷單晶矽的生產。 A production method of phosphorus-doped monocrystalline silicon to avoid dust explosion, which is characterized in that it comprises the following steps: The raw material polycrystalline silicon is added to the main chamber of the single crystal furnace, and a vacuum is formed in the furnace and the inert gas is passed through the dust-proof vacuum method in the production of phosphorus-doped single crystal silicon as described in any one of Claims 1 to 6. After heating the raw material to melt it, the crystal will start to grow for the production of phosphorus-doped single crystal silicon.
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