TWI658002B - Method of manufacturing silicon monoxide deposit and manufacturing equipment implementing such method - Google Patents

Method of manufacturing silicon monoxide deposit and manufacturing equipment implementing such method Download PDF

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TWI658002B
TWI658002B TW107128497A TW107128497A TWI658002B TW I658002 B TWI658002 B TW I658002B TW 107128497 A TW107128497 A TW 107128497A TW 107128497 A TW107128497 A TW 107128497A TW I658002 B TWI658002 B TW I658002B
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silicon
powders
cooling jacket
powder
core composite
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TW107128497A
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TW202009215A (en
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藍崇文
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國立臺灣大學
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Abstract

一種製造一氧化矽沉積物之方法及執行該方法之製造設備。根據本發明之方法係採用多顆二氧化矽殼/矽核複合粉體而非採用矽粉體與二氧化矽粉體來反應成一氧化矽並昇華為一氧化矽蒸氣,再收集一氧化矽蒸氣將其冷卻成一氧化矽沉積物。 A method for manufacturing a silicon oxide deposit and manufacturing equipment for performing the method. The method according to the present invention uses multiple silicon dioxide shell / silicon core composite powders instead of using silicon powders and silicon dioxide powders to react to silicon oxide and sublimate it into silicon monoxide vapor, and then collects silicon monoxide vapor It is cooled to a silicon oxide deposit.

Description

製造一氧化矽沉積物之方法及執行該方法之製造設備 Method for manufacturing silicon monoxide deposit and manufacturing equipment for carrying out the method

本發明係關於一種製造一氧化矽沉積物之方法及執行該方法之製造設備,並且特別地,關於不採用矽粉體與二氧化矽粉體來製造一氧化矽沉積物之方法及執行該方法之製造設備。 The present invention relates to a method for manufacturing a silicon monoxide deposit and a manufacturing device for performing the method, and in particular, to a method for manufacturing a silicon monoxide deposit without using a silicon powder and a silicon dioxide powder, and to execute the method Manufacturing equipment.

一氧化矽粉體是一種廣泛用於光學玻璃鍍膜和製作半導體的材料。例如,照明燈具、眼鏡、光學鏡頭、寶石、玩具等鍍膜以及IC產業的重要原料之一。一氧化矽的光學應用方面,可做為抗反射塗層、吸收塗層、保護塗層等。一氧化矽可做為用於液晶導電膜的保護絕緣塗層。一氧化矽可做為用於半導體元件的保護絕緣塗層。一氧化矽可做為用於薄膜電容器的介電層。一氧化矽可做為用於太陽能電池的抗反射塗層。一氧化矽可做為用於阻氣膜的沉積材料。一氧化矽可以用於鋰離子充電電池的負極材料 Silicon monoxide powder is a widely used material for optical glass coating and semiconductor manufacturing. For example, coatings for lighting fixtures, glasses, optical lenses, gems, toys and other important raw materials for the IC industry. For optical applications of silicon oxide, it can be used as anti-reflective coating, absorption coating, protective coating, etc. Silicon monoxide can be used as a protective insulating coating for liquid crystal conductive films. Silicon monoxide can be used as a protective insulating coating for semiconductor components. Silicon oxide can be used as a dielectric layer for thin film capacitors. Silicon monoxide can be used as an anti-reflection coating for solar cells. Silicon monoxide can be used as a deposition material for a gas barrier film. Silicon monoxide can be used as a negative electrode material for lithium ion rechargeable batteries

關於一氧化矽之製造方法的先前技術,請參閱中國大陸專利公開號1451057A以及美國專利公告號7,431,899B2。這些先前技術揭示將矽粉體與二氧化矽粉體混合,置於高溫下讓矽粉體與二氧化矽粉體反應成一氧化矽並昇華為一氧化矽蒸氣,再收集一氧化矽蒸氣將其冷卻成一氧化矽沉積物。 For the prior art of the manufacturing method of silicon monoxide, please refer to Mainland China Patent Publication No. 1451057A and US Patent Publication No. 7,431,899B2. These previous techniques revealed that mixing silicon powder with silicon dioxide powder, and placing silicon powder and silicon dioxide powder at high temperature to react with silicon oxide and sublimate it into silicon monoxide vapor, and then collect silicon monoxide vapor to separate it Cool to a silicon oxide deposit.

然而,二氧化矽粉體的比表面積可高達400-600 m2/g之譜,矽粉體的比表面積則為3m2/g。美國專利公告號7,431,899 B2中之一範例即揭示二氧化矽粉體的比表面積可高達200m2/g,矽粉體的比表面積為3m2/g,若以粒徑為40nm的二氧化矽粉體與矽粉體混合在一起做為原料,其混合物整體的密度為0.25g/cm3。因此,單位重量的二氧化矽粉體與矽粉體混合粉體佔據空間較大,加熱上也較為耗能。 However, the specific surface area of silicon dioxide powder can be as high as 400-600 m 2 / g, and the specific surface area of silicon powder is 3 m 2 / g. One example of U.S. Patent Publication No. 7,431,899 B2 is that the specific surface area of silicon dioxide powder can be as high as 200 m 2 / g, and the specific surface area of silicon powder is 3 m 2 / g. And silicon powder are mixed together as a raw material, and the overall density of the mixture is 0.25 g / cm 3 . Therefore, the mixed powder of silicon dioxide powder and silicon powder per unit weight occupies a larger space and consumes more energy in heating.

此外,因為在加熱室中進行的矽粉體與二氧化矽粉體的反應是固相反應,所以前述接觸面積控制反應速度。因此,接觸面積越小,反應速度越慢,單位時間內的沉積量會減少。 In addition, since the reaction between the silicon powder and the silicon dioxide powder in the heating chamber is a solid phase reaction, the aforementioned contact area controls the reaction speed. Therefore, the smaller the contact area, the slower the reaction rate, and the less the amount of deposition per unit time.

目前尚缺乏不採用矽粉體與二氧化矽粉體的反應成一氧化矽的方法,以縮減加熱室空間,降低耗能。 At present, there is still a lack of a method for forming silicon monoxide without using the reaction between silicon powder and silicon dioxide powder to reduce the space of the heating chamber and reduce energy consumption.

此外,先前技術之製造一氧化矽沉積物的設備,整體佔據空間皆龐大,不僅僅較大的加熱空間較為耗能,其冷卻設計也存有改善的空間。 In addition, the equipment for manufacturing silicon oxide deposits in the prior art has a large overall space. Not only does the larger heating space consume more energy, but its cooling design also has room for improvement.

因此,本發明所欲解決之一技術問題在於提供一種不採用矽粉體與二氧化矽粉體來製造一氧化矽沉積物之方法及執行該方法之製造設備。根據本發明之方法之單位時間內的產能較高。根據本發明之製造設備之整體體積較小,且較不耗能,單位時間內的產能較高。 Therefore, one technical problem to be solved by the present invention is to provide a method for manufacturing a silicon oxide deposit without using a silicon powder and a silicon dioxide powder, and a manufacturing equipment for performing the method. The method according to the present invention has a higher capacity per unit time. The overall volume of the manufacturing equipment according to the present invention is smaller, and it consumes less energy, and the production capacity per unit time is higher.

本發明之第一較佳具體實施例之製造一氧化矽沉積物之方法,首先係製備複數顆矽粉體。接著,本發明之方法係將複數顆矽粉體加熱至第一溫度且維持一加熱時間,致使每一顆矽粉體表面形成二氧化矽層。多顆矽粉體變成多顆二氧化矽殼/矽核複合粉體。接著,本發明之方法係將多顆二氧化矽殼/矽核複合粉體置於真空環境或鈍態氣氛中且加熱至第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化 矽殼與矽核反應成一氧化矽且昇華成一氧化矽蒸氣。最後,本發明之方法係收集且冷卻一氧化矽蒸氣,即獲得一氧化矽沉積物。 The method for manufacturing a silicon oxide deposit according to the first preferred embodiment of the present invention is to first prepare a plurality of silicon powders. Next, the method of the present invention heats a plurality of silicon powders to a first temperature and maintains a heating time, so that a silicon dioxide layer is formed on the surface of each silicon powder. Multiple silicon powders become multiple silicon dioxide shell / silicon composite powders. Next, in the method of the present invention, a plurality of silicon dioxide shell / silicon core composite powders are placed in a vacuum environment or a passive atmosphere and heated to a second temperature, so that each silicon dioxide shell / silicon core composite powder is Dioxide The silicon shell reacts with the silicon core to form silicon monoxide and sublimates into silicon monoxide vapor. Finally, the method of the present invention collects and cools silicon monoxide vapor to obtain silicon monoxide deposits.

於一具體實施例中,多顆二氧化矽殼/矽核複合粉體之Si/SO2莫耳數比例範圍為從0.8至1.2。 In a specific embodiment, the Si / SO 2 mole number ratio of the plurality of silica dioxide / silicon core composite powders ranges from 0.8 to 1.2.

於一具體實施例中,第一溫度之範圍為從600℃至900℃。 In a specific embodiment, the first temperature ranges from 600 ° C to 900 ° C.

於一具體實施例中,第二溫度之範圍為從1200℃至1450℃。 In a specific embodiment, the second temperature ranges from 1200 ° C to 1450 ° C.

本發明之第二較佳具體實施例之製造一氧化矽沉積物之方法,首先係製備複數顆第一矽粉體。接著,本發明之方法係將複數顆第一矽粉體加熱至第一溫度且維持一加熱時間,致使每一顆第一矽粉體表面形成二氧化矽層。多顆第一矽粉體變成多顆二氧化矽殼/矽核複合粉體。接著,本發明之方法係將多顆二氧化矽殼/矽核複合粉體與多顆第二矽粉體置於真空環境或鈍態氣氛中且加熱至第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一氧化矽蒸氣。最後,本發明之方法係收集且冷卻一氧化矽蒸氣,即獲得一氧化矽沉積物。 The method for manufacturing a silicon oxide deposit according to the second preferred embodiment of the present invention is to first prepare a plurality of first silicon powders. Then, the method of the present invention heats a plurality of first silicon powders to a first temperature and maintains a heating time, so that a silicon dioxide layer is formed on the surface of each first silicon powder. Multiple first silicon powders become multiple silicon dioxide shell / silicon core composite powders. Next, in the method of the present invention, a plurality of silicon dioxide shell / silicon core composite powders and a plurality of second silicon powders are placed in a vacuum environment or a passive atmosphere and heated to a second temperature, so that each of them The silica shell of the silicon shell / silicon core composite powder reacts with the silicon core and each second silicon powder to form silicon monoxide and sublimates into silicon monoxide vapor. Finally, the method of the present invention collects and cools silicon monoxide vapor to obtain silicon monoxide deposits.

本發明之第一較佳具體實施例之製造設備包含爐體、冷卻夾套、至少一沉積基板以及真空抽氣裝置。複數顆第一矽粉體係置於爐體內。冷卻夾套係安置於爐體之第一頂部上,並且與爐體之第一頂部連通。冷卻夾套具有儲液腔、液體入口以及液體出口。至少一沉積基板係放置於冷卻夾套內,並且與冷卻夾套之內壁熱耦合。真空抽氣裝置係與冷卻夾套之第二頂部連通。爐體將複數顆第一矽粉體加熱至第一溫度且維持一加熱時間,致使每一顆第一矽粉體表面形成二 氧化矽層。多顆第一矽粉體變成多顆二氧化矽殼/矽核複合粉體。真空抽氣裝置接著持續運作將爐體內以及冷卻夾套內形成真空環境。爐體接著將多顆二氧化矽殼/矽核複合粉體或將多顆二氧化矽殼/矽核複合粉體與新添加的複數顆第二矽粉體一起加熱至第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核反應或每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一氧化矽蒸氣。冷卻液體從冷卻夾套之液體入口流入冷卻夾套之儲液腔從冷卻夾套之液體出口流出,讓至少一沉積基板之溫度低於第三溫度,致使流經冷卻夾套內之一氧化矽蒸氣沉積於至少一沉積基板上形成一氧化矽沉積物。 The manufacturing equipment of the first preferred embodiment of the present invention includes a furnace body, a cooling jacket, at least one deposition substrate, and a vacuum extraction device. A plurality of first silicon powder systems are placed in the furnace. The cooling jacket is arranged on the first top of the furnace body and communicates with the first top of the furnace body. The cooling jacket has a liquid storage cavity, a liquid inlet and a liquid outlet. At least one deposition substrate is placed in the cooling jacket and is thermally coupled to the inner wall of the cooling jacket. The vacuum extraction device is in communication with the second top of the cooling jacket. The furnace body heats a plurality of first silicon powders to a first temperature and maintains a heating time, so that the surface of each first silicon powder forms two Silicon oxide layer. Multiple first silicon powders become multiple silicon dioxide shell / silicon core composite powders. The vacuum extraction device continues to operate to form a vacuum environment inside the furnace and the cooling jacket. The furnace body then heats multiple silicon dioxide shells / silicon core composite powders or multiple silicon dioxide shells / silicon core composite powders with the newly added plurality of second silicon powders to a second temperature, so that each One silicon dioxide shell / silicon core composite powder of silicon dioxide shell and silicon core reaction or each silicon dioxide shell / silicon core composite powder of silicon dioxide shell and silicon core and each second silicon powder The body reacts to silicon monoxide and sublimates into silicon monoxide vapor. The cooling liquid flows from the liquid inlet of the cooling jacket into the liquid storage cavity of the cooling jacket and flows out of the liquid outlet of the cooling jacket, so that the temperature of at least one deposition substrate is lower than the third temperature, causing a silicon oxide flowing through the cooling jacket Vapor deposition is performed on at least one deposition substrate to form a silicon oxide deposit.

進一步,根據本發明之製造設備還包含第一檔板。第一檔板係安置於至少一沉積基板所圍成之空間的上方。一氧化矽蒸氣也沉積於第一檔板上。 Further, the manufacturing apparatus according to the present invention further includes a first baffle. The first baffle plate is disposed above the space surrounded by the at least one deposition substrate. Silicon monoxide vapor is also deposited on the first baffle.

進一步,根據本發明之製造設備還包含第二檔板。真空抽氣裝置係以導管與冷卻夾套之第二頂部連通。第二檔板係安置於冷卻夾套內靠近導管以阻擋一氧化矽蒸氣被抽出冷卻夾套。 Further, the manufacturing apparatus according to the present invention further includes a second baffle. The vacuum pumping device is connected to the second top of the cooling jacket by a duct. The second baffle plate is arranged in the cooling jacket near the duct to prevent the silicon oxide vapor from being drawn out of the cooling jacket.

本發明之第二較佳具體實施例之製造設備包含爐體、冷卻夾套、至少一沉積基板以及鈍態氣體供應裝置。複數顆第一矽粉體係置於爐體內。冷卻夾套係安置於爐體之第一頂部上,並且與爐體之第一頂部連通。冷卻夾套具有儲液腔、液體入口以及液體出口。至少一沉積基板係放置於冷卻夾套內,並且與冷卻夾套之內壁熱耦合。鈍態氣體供應裝置係與冷卻夾套之第二頂部連通。爐體將複數顆第一矽粉體加熱至第一溫度且維持一加熱時間,致使每一顆第一矽粉體表面形成二氧化矽層。多顆第一矽粉體變成多顆二氧化矽殼/矽核複合粉體。鈍態氣體供應裝置接著持續運作供應鈍態氣體將爐體內以及冷卻夾套內形成鈍態氣氛。爐體接著將多顆 二氧化矽殼/矽核複合粉體或將多顆二氧化矽殼/矽核複合粉體與新添加的複數顆第二矽粉體一起加熱至第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核反應或每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一氧化矽蒸氣。冷卻液體從冷卻夾套之液體入口流入冷卻夾套之儲液腔從冷卻夾套之液體出口流出,讓至少一沉積基板之溫度低於第三溫度,致使流經冷卻夾套內之一氧化矽蒸氣沉積於至少一沉積基板上形成一氧化矽沉積物。 The manufacturing equipment of the second preferred embodiment of the present invention includes a furnace body, a cooling jacket, at least one deposition substrate, and a passive gas supply device. A plurality of first silicon powder systems are placed in the furnace. The cooling jacket is arranged on the first top of the furnace body and communicates with the first top of the furnace body. The cooling jacket has a liquid storage cavity, a liquid inlet and a liquid outlet. At least one deposition substrate is placed in the cooling jacket and is thermally coupled to the inner wall of the cooling jacket. The passive gas supply device is in communication with the second top of the cooling jacket. The furnace body heats the plurality of first silicon powders to a first temperature and maintains a heating time, so that a silicon dioxide layer is formed on the surface of each of the first silicon powders. Multiple first silicon powders become multiple silicon dioxide shell / silicon core composite powders. The passive gas supply device then continues to operate to supply a passive gas to form a passive atmosphere in the furnace and the cooling jacket. The furnace body will then Silicon dioxide shell / silicon core composite powder or heating multiple silicon dioxide shell / silicon core composite powders with newly added plurality of second silicon powders to a second temperature, resulting in each silicon dioxide shell The silicon dioxide shell of the / silicon core composite powder reacts with the silicon core or the silicon dioxide shell of each silicon dioxide shell / silicon core composite powder reacts with the silicon core and each second silicon powder to form silicon monoxide and Sublimation into silicon monoxide vapor. The cooling liquid flows from the liquid inlet of the cooling jacket into the liquid storage cavity of the cooling jacket and flows out of the liquid outlet of the cooling jacket, so that the temperature of at least one deposition substrate is lower than the third temperature, causing a silicon oxide flowing through the cooling jacket Vapor deposition is performed on at least one deposition substrate to form a silicon oxide deposit.

與先前技術不同,本發明之方法不採用矽粉體與二氧化矽粉體來製造一氧化矽沉積物。執行本發明之方法的製造設備,其整體體積較小,且較不耗能,單位時間內的產能較高。 Unlike the prior art, the method of the present invention does not use silicon powder and silicon dioxide powder to make silicon monoxide deposits. The manufacturing equipment for implementing the method of the present invention has a smaller overall volume and less energy consumption, and has a higher productivity per unit time.

關於本發明之優點與精神可以藉由以下的發明詳述及所附圖式得到進一步的瞭解。 The advantages and spirit of the present invention can be further understood through the following detailed description of the invention and the accompanying drawings.

1‧‧‧方法 1‧‧‧method

S10~S16‧‧‧流程步驟 S10 ~ S16‧‧‧Process steps

2‧‧‧方法 2‧‧‧Method

S20~S26‧‧‧流程步驟 S20 ~ S26‧‧‧Process steps

3‧‧‧製造設備 3‧‧‧ manufacturing equipment

30‧‧‧爐體 30‧‧‧furnace

300‧‧‧通孔 300‧‧‧through hole

302‧‧‧第一頂部 302‧‧‧First top

304‧‧‧座體 304‧‧‧ seat

306‧‧‧加熱器 306‧‧‧heater

32‧‧‧冷卻夾套 32‧‧‧cooling jacket

322‧‧‧第二頂部 322‧‧‧second top

324‧‧‧儲液腔 324‧‧‧Storage chamber

326‧‧‧液體入口 326‧‧‧Liquid inlet

328‧‧‧液體出口 328‧‧‧Liquid outlet

34‧‧‧沉積基板 34‧‧‧ Deposition substrate

342‧‧‧空間 342‧‧‧Space

36‧‧‧真空抽氣裝置 36‧‧‧Vacuum extraction device

362‧‧‧導管 362‧‧‧catheter

37‧‧‧第一檔板 37‧‧‧First baffle

38‧‧‧第二檔板 38‧‧‧Second baffle

39‧‧‧鈍態氣體供應裝置 39‧‧‧ Passive gas supply device

40‧‧‧第一矽粉體 40‧‧‧The first silicon powder

42‧‧‧二氧化矽殼/矽核複合粉體 42‧‧‧Silica dioxide / silicon core composite powder

44‧‧‧一氧化矽蒸氣 44‧‧‧Silicon monoxide vapor

46‧‧‧一氧化矽沉積物 46‧‧‧Silica oxide deposits

5‧‧‧坩堝 5‧‧‧ Crucible

L‧‧‧冷卻液體 L‧‧‧ cooling liquid

圖1係本發明之第一較佳具體實施例之方法的各個程序步驟流程圖。 FIG. 1 is a flowchart of each program step of the method of the first preferred embodiment of the present invention.

圖2係本發明之第二較佳具體實施例之方法的各個程序步驟流程圖。 FIG. 2 is a flowchart of each program step of the method of the second preferred embodiment of the present invention.

圖3係本發明之第一較佳具體實施例之製造設備的架構之示意圖。 FIG. 3 is a schematic diagram of the structure of the manufacturing equipment of the first preferred embodiment of the present invention.

圖4及圖5係圖3所示製造設備處於製造一氧化矽沉積物不同階段的示意圖。 4 and 5 are schematic diagrams of the manufacturing equipment shown in FIG. 3 at different stages of manufacturing silicon oxide deposits.

圖6係本發明之第二較佳具體實施例之製造設備的架構之示意圖。 FIG. 6 is a schematic diagram of a structure of a manufacturing apparatus according to a second preferred embodiment of the present invention.

圖7及圖8係圖6所示製造設備處於製造一氧化矽沉積物不同階段的示意圖。 FIG. 7 and FIG. 8 are schematic diagrams of the manufacturing equipment shown in FIG. 6 at different stages of manufacturing silicon oxide deposits.

請參閱圖1,為根據本發明之第一較佳具體實施例之方法1之流程圖。根據本發明之較佳具體實施例之方法1不採用先前技術所採用的矽粉體與二氧化矽粉體來製造一氧化矽沉積物。 Please refer to FIG. 1, which is a flowchart of a method 1 according to a first preferred embodiment of the present invention. Method 1 according to a preferred embodiment of the present invention does not use the silicon powder and the silicon dioxide powder used in the prior art to manufacture the silicon monoxide deposit.

如圖1所示,本發明之方法1,首先係執行步驟S10,製備複數顆矽粉體。 As shown in FIG. 1, the method 1 of the present invention first executes step S10 to prepare a plurality of silicon powders.

於實際應用中,複數顆矽粉體可以採用回收自矽泥之高純度矽粉體。矽泥即為運用線切割技術切削矽晶棒、矽晶鑄錠而得,矽泥的成份包含有機質、金屬物質、多個矽粉末以及多個碳化矽粉末。已有先前技術可以從矽泥中回收純度甚高的矽,在此不做贅述。 In practical applications, the plurality of silicon powders can be high-purity silicon powders recovered from silicon mud. Silicon mud is obtained by cutting silicon rods and silicon ingots using wire cutting technology. The composition of silicon mud includes organic matter, metal substances, multiple silicon powders and multiple silicon carbide powders. Existing technologies can recover very pure silicon from silicon mud, which is not described in detail here.

接著,本發明之方法1係執行步驟S12,將複數顆矽粉體加熱至第一溫度且維持一加熱時間,致使每一顆矽粉體表面形成二氧化矽層。特別地,多顆矽粉體變成多顆二氧化矽殼/矽核複合粉體。 Next, the method 1 of the present invention executes step S12 to heat a plurality of silicon powders to a first temperature and maintain a heating time, so that a silicon dioxide layer is formed on the surface of each silicon powder. In particular, multiple silicon powders become multiple silicon dioxide shell / silicon core composite powders.

於一具體實施例中,第一溫度之範圍為從600℃至900℃。 In a specific embodiment, the first temperature ranges from 600 ° C to 900 ° C.

於一範例中,複數顆矽粉體之平均粒徑為1微米。複數顆矽粉體加熱至700℃,且維持12至36小時,進行除碳以及後續的表面氧化。多顆二氧化矽殼/矽核複合粉體之Si/SO2莫耳數比例範圍為從0.8至1.2。 In one example, the average particle size of the plurality of silicon powders is 1 micron. The plurality of silicon powders are heated to 700 ° C. and maintained for 12 to 36 hours for carbon removal and subsequent surface oxidation. The Si / SO 2 mole ratio of multiple silica dioxide / silicon core powders ranges from 0.8 to 1.2.

接著,本發明之方法1係執行步驟S14,將多顆二氧化矽殼/矽核複合粉體置於真空環境且加熱至第二溫度, 致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核反應成一氧化矽且昇華成一氧化矽蒸氣。 Next, the method 1 of the present invention executes step S14, placing a plurality of silicon dioxide shell / silicon core composite powders in a vacuum environment and heating to a second temperature, As a result, the silicon dioxide shell of each silicon dioxide shell / silicon core composite powder reacts with the silicon core to form silicon monoxide and sublimates into silicon monoxide vapor.

於一具體實施例中,第二溫度之範圍為從1200℃至1450℃。 In a specific embodiment, the second temperature ranges from 1200 ° C to 1450 ° C.

於一具體實施例中,真空環境的真空度為小於1torr。 In a specific embodiment, the vacuum degree of the vacuum environment is less than 1 torr.

最後,本發明之方法係執行步驟S16,收集且冷卻一氧化矽蒸氣,即獲得一氧化矽沉積物。 Finally, the method of the present invention executes step S16 to collect and cool the silicon oxide vapor to obtain a silicon oxide deposit.

請參閱圖2,為根據本發明之第二較佳具體實施例之方法2之流程圖。根據本發明之較佳具體實施例之方法2不採用先前技術所採用的矽粉體與二氧化矽粉體來製造一氧化矽沉積物。 Please refer to FIG. 2, which is a flowchart of a method 2 according to a second preferred embodiment of the present invention. The method 2 according to a preferred embodiment of the present invention does not use the silicon powder and the silicon dioxide powder used in the prior art to manufacture silicon monoxide deposits.

如圖2所示,本發明之方法1,首先係執行步驟S20,製備複數顆第一矽粉體。 As shown in FIG. 2, method 1 of the present invention first executes step S20 to prepare a plurality of first silicon powders.

於實際應用中,同樣地,複數顆第一矽粉體可以採用回收自矽泥之高純度的矽粉體。 In practical applications, similarly, the plurality of first silicon powders can be high-purity silicon powders recovered from silicon mud.

接著,本發明之方法2係執行步驟S22,將複數顆第一矽粉體加熱至第一溫度且維持一加熱時間,致使每一顆第一矽粉體表面形成二氧化矽層。特別地,多顆第一矽粉體變成多顆二氧化矽殼/矽核複合粉體。 Next, the method 2 of the present invention executes step S22, heating a plurality of first silicon powders to a first temperature and maintaining a heating time, so that a silicon dioxide layer is formed on the surface of each first silicon powder. In particular, the plurality of first silicon powders becomes a plurality of silicon dioxide shell / silicon core composite powders.

於一具體實施例中,第一溫度之範圍為從600℃至900℃。 In a specific embodiment, the first temperature ranges from 600 ° C to 900 ° C.

於一範例中,複數顆第一矽粉體之平均粒徑為1微米。複數顆第一矽粉體加熱至700℃,且維持12至36小時,進行除碳以及後續的表面氧化。 In one example, the average particle size of the plurality of first silicon powders is 1 micron. The plurality of first silicon powders are heated to 700 ° C. and maintained for 12 to 36 hours for carbon removal and subsequent surface oxidation.

接著,本發明之方法2係執行步驟S24,將多顆 二氧化矽殼/矽核複合粉體與多顆第二矽粉體置於真空環境且加熱至第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一氧化矽蒸氣。多顆二氧化矽殼/矽核複合粉體與多顆第二矽粉體之Si/SO2莫耳數比例範圍為從0.8至1.2。同樣地,複數顆第二矽粉體可以採用回收自矽泥之高純度的矽粉體。 Next, the method 2 of the present invention executes step S24, placing a plurality of silicon dioxide shell / silicon core composite powders and a plurality of second silicon powders in a vacuum environment and heating to a second temperature, so that each of the two dioxides The silica shell of the silicon shell / silicon core composite powder reacts with the silicon core and each second silicon powder to form silicon monoxide and sublimates into silicon monoxide vapor. The ratio of the Si / SO 2 mole number of the plurality of silicon dioxide shell / silicon core powders to the plurality of second silicon powders ranges from 0.8 to 1.2. Similarly, the plurality of second silicon powders may be high-purity silicon powders recovered from silicon mud.

於一具體實施例中,第二溫度之範圍為從1200℃至1450℃。 In a specific embodiment, the second temperature ranges from 1200 ° C to 1450 ° C.

於一具體實施例中,真空環境的真空度為小於1torr。 In a specific embodiment, the vacuum degree of the vacuum environment is less than 1 torr.

最後,本發明之方法係執行步驟S16,收集且冷卻一氧化矽蒸氣,即獲得一氧化矽沉積物。 Finally, the method of the present invention executes step S16 to collect and cool the silicon oxide vapor to obtain a silicon oxide deposit.

請參閱圖3,圖3係示意地繪示本發明之第一較佳具體實施例之製造設備3的架構。於圖3中,部分元件及裝置係以剖面視圖顯示。 Please refer to FIG. 3. FIG. 3 schematically illustrates the structure of the manufacturing equipment 3 of the first preferred embodiment of the present invention. In FIG. 3, some components and devices are shown in a cross-sectional view.

如圖3所示,根據本發明之第一較佳具體實施例之製造設備3包含爐體30、冷卻夾套32、至少一沉積基板34以及真空抽氣裝置36。 As shown in FIG. 3, the manufacturing equipment 3 according to the first preferred embodiment of the present invention includes a furnace body 30, a cooling jacket 32, at least one deposition substrate 34, and a vacuum extraction device 36.

爐體30包含熱絕緣的座體304以及至少一加熱器306。於一具體實施例中,座體304可以由碳纖維所製成,但並不以此為限。 The furnace body 30 includes a thermally insulated base body 304 and at least one heater 306. In a specific embodiment, the base 304 may be made of carbon fiber, but is not limited thereto.

冷卻夾套32係安置於爐體30之第一頂部302上,並且與爐體30之第一頂部302連通。例如,如圖3所示,爐體30之第一頂部302上具有複數個通孔300。複數個通孔300讓冷卻夾套32與爐體30之第一頂部302連通。 The cooling jacket 32 is disposed on the first top portion 302 of the furnace body 30 and communicates with the first top portion 302 of the furnace body 30. For example, as shown in FIG. 3, the first top portion 302 of the furnace body 30 has a plurality of through holes 300. The plurality of through holes 300 allow the cooling jacket 32 to communicate with the first top portion 302 of the furnace body 30.

冷卻夾套32具有儲液腔324、液體入口326以及液體出口328。冷卻液體L從冷卻夾套32之液體入口326 流入冷卻夾套32之儲液腔324從冷卻夾套32之液體出口328流出。 The cooling jacket 32 has a liquid storage cavity 324, a liquid inlet 326, and a liquid outlet 328. Cooling liquid L from liquid inlet 326 of cooling jacket 32 The liquid storage cavity 324 flowing into the cooling jacket 32 flows out from the liquid outlet 328 of the cooling jacket 32.

至少一沉積基板34係放置於冷卻夾套32內,並且與冷卻夾套32之內壁熱耦合。真空抽氣裝置36係與冷卻夾套32之第二頂部322連通。 At least one deposition substrate 34 is placed in the cooling jacket 32 and is thermally coupled to the inner wall of the cooling jacket 32. The vacuum extraction device 36 is in communication with the second top portion 322 of the cooling jacket 32.

請再參閱圖3及圖4、圖5,利用根據本發明之第一較佳具體實施例之製造設備3製造一氧化矽沉積物46如下文所述。 Please refer to FIG. 3, FIG. 4 and FIG. 5 again, and use the manufacturing equipment 3 according to the first preferred embodiment of the present invention to manufacture the silicon oxide deposit 46 as described below.

如圖3所示,首先,複數顆矽粉體40係置於坩堝5內,再將盛裝複數顆第一矽粉體40的坩堝5置於爐體30內,至少一加熱器306圍繞在坩堝5的外壁。於一具體實施例中,坩堝5可以由石墨所製成,但並不以此為限。 As shown in FIG. 3, first, a plurality of silicon powders 40 are placed in the crucible 5, and then the crucible 5 containing the plurality of first silicon powders 40 is placed in the furnace body 30. At least one heater 306 surrounds the crucible 5 outer walls. In a specific embodiment, the crucible 5 may be made of graphite, but is not limited thereto.

如圖4所示,接著,爐體30將複數顆第一矽粉體40加熱至第一溫度且維持一加熱時間,致使每一顆第一矽粉體40表面形成二氧化矽層。多顆矽粉體40變成多顆二氧化矽殼/矽核複合粉體42。第一溫度之範圍以及多顆二氧化矽殼/矽核複合粉體之Si/SO2比例範圍如上文所述,在此不再贅述。 As shown in FIG. 4, the furnace body 30 heats the plurality of first silicon powder bodies 40 to a first temperature and maintains a heating time, so that a silicon dioxide layer is formed on the surface of each of the first silicon powder bodies 40. The plurality of silicon powders 40 become a plurality of silicon dioxide shell / silicon core composite powders 42. The range of the first temperature and the range of the Si / SO 2 ratio of the plurality of silicon dioxide shell / silicon core powders are as described above, and are not repeated here.

如圖5所示,接著,真空抽氣裝置36接著持續運作將爐體30內以及冷卻夾套32內形成真空環境。爐體30接著將多顆二氧化矽殼/矽核複合粉體42或將多顆二氧化矽殼/矽核複合粉體42與新添加的複數顆第二矽粉體(未繪示於圖中)一起加熱至第二溫度,致使每一顆二氧化矽殼/矽核複合粉體42的二氧化矽殼與矽核或每一顆二氧化矽殼/矽核複合粉體42的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一氧化矽蒸氣44。一氧化矽蒸氣44經過通孔300,流入冷卻夾套32內。通孔300還可以避免二氧化矽殼/矽核複合粉體42飛濺進入冷卻夾套32內。 As shown in FIG. 5, the vacuum extraction device 36 continues to operate to form a vacuum environment in the furnace body 30 and the cooling jacket 32. The furnace body 30 then combines a plurality of silicon dioxide shells / silicon core composite powders 42 or a plurality of silicon dioxide shells / silicon core composite powders 42 with newly added plurality of second silicon powders (not shown in the figure) Middle) together to the second temperature, causing the silica dioxide of each silica shell / silicon core composite powder 42 and the silica or the silica of each silica shell / silicon core composite powder 42 The silicon shell reacts with the silicon core and each second silicon powder to form silicon oxide and sublimate into silicon oxide vapor 44. Silicon monoxide vapor 44 flows through the through hole 300 and flows into the cooling jacket 32. The through hole 300 can also prevent the silicon dioxide shell / silicon core composite powder 42 from splashing into the cooling jacket 32.

冷卻液體L持續從冷卻夾套32之液體入口326流入冷卻夾套32之儲液腔324從冷卻夾套32之液體出口328流出,讓至少一沉積基板34之溫度低於第三溫度,致使流經冷卻夾套32內之一氧化矽蒸氣44沉積於至少一沉積基板34上形成一氧化矽沉積物46。第二溫度之範圍以及真空環境的真空度如上文所述,在此不再贅述。 The cooling liquid L continuously flows from the liquid inlet 326 of the cooling jacket 32 into the liquid storage cavity 324 of the cooling jacket 32 and flows out of the liquid outlet 328 of the cooling jacket 32, so that the temperature of at least one deposition substrate 34 is lower than the third temperature, causing A silicon oxide vapor 44 in the cooling jacket 32 is deposited on at least one deposition substrate 34 to form a silicon oxide deposit 46. The range of the second temperature and the degree of vacuum of the vacuum environment are as described above, and are not repeated here.

於一具體實施例中,冷卻液體L可以是水,但並不以此為限。 In a specific embodiment, the cooling liquid L may be water, but is not limited thereto.

於一具體實施例中,第三溫度為400℃。 In a specific embodiment, the third temperature is 400 ° C.

進一步,同樣如圖3所示,根據本發明之第一較佳具體之實施例之製造設備3還包含第一檔板37。第一檔板37係安置於至少一沉積基板34所圍成之空間342的上方。一氧化矽蒸氣46也沉積於第一檔板37上。 Further, as shown in FIG. 3, the manufacturing equipment 3 according to the first preferred embodiment of the present invention further includes a first baffle plate 37. The first baffle plate 37 is disposed above the space 342 surrounded by the at least one deposition substrate 34. Silicon monoxide vapor 46 is also deposited on the first baffle plate 37.

進一步,同樣如圖3所示,根據本發明之第一較佳具體實施例之製造設備3還包含第二檔板38。真空抽氣裝置36係以導管362與冷卻夾套32之第二頂部322連通。第二檔板38係安置於冷卻夾套32內靠近導管362以阻擋一氧化矽蒸氣46被抽出冷卻夾套32。 Further, as shown in FIG. 3, the manufacturing apparatus 3 according to the first preferred embodiment of the present invention further includes a second baffle plate 38. The vacuum pumping device 36 is in communication with the second top portion 322 of the cooling jacket 32 through a duct 362. The second baffle plate 38 is disposed in the cooling jacket 32 near the duct 362 to prevent the silicon oxide vapor 46 from being drawn out of the cooling jacket 32.

於一氧化矽沉積物46製造完成後,至少一沉積基板34以及第一檔板37可以自冷卻夾套32內取出,收取一氧化矽沉積物46。根據本發明之方法所製造的一氧化矽沉積物46為黑色的沉積物。 After the silicon oxide deposit 46 is manufactured, at least one deposition substrate 34 and the first baffle plate 37 can be taken out of the cooling jacket 32 to collect the silicon oxide deposit 46. The silicon oxide deposit 46 produced according to the method of the present invention is a black deposit.

於一範例中,1kg的矽粉體經氧化成二氧化矽殼/矽核複合粉體,二氧化矽殼/矽核複合粉體整體密度約為0.656g/cm3。再根據本發明之方法所製造的一氧化矽沉積物,約經6小時,可產出產率大於90%的一氧化矽黑色沉積物。 In one example, 1 kg of silicon powder is oxidized into a silicon dioxide shell / silicon core composite powder, and the overall density of the silicon dioxide shell / silicon core powder is about 0.656 g / cm 3 . The silicon monoxide deposit produced according to the method of the present invention can produce a silicon monoxide black deposit with a yield of more than 90% in about 6 hours.

與先前技術相比較,先前技術若以粒徑為40nm 的二氧化矽粉體與矽粉體混合在一起做為原料,其混合物整體的密度為0.25g/cm3。若原料是先前技術所採用整體密度為0.25g/cm3混合粉體物,其所需加熱空間為本發明所採用整體密度約為0.656g/cm3的二氧化矽殼/矽核複合粉體之2.5倍。顯見地,根據本發明方法製造一氧化矽沉積物所耗的能量較低。 Compared with the prior art, if the prior art uses silicon dioxide powder with a particle size of 40 nm and silicon powder as a raw material, the overall density of the mixture is 0.25 g / cm 3 . If prior art materials are used the bulk density of 0.25g / cm 3 mixed powder was heated space which is required for the present invention is employed in the overall density of about 0.656g / cm 3 of silicon dioxide shell / silica core composite powder 2.5 times. Obviously, the energy consumed to make the silicon monoxide deposits according to the method of the invention is lower.

請參閱圖6,圖6係示意地繪示本發明之第二較佳具體實施例之製造設備3的架構。於圖6中,部分元件及裝置係以剖面視圖顯示。 Please refer to FIG. 6. FIG. 6 schematically illustrates the structure of the manufacturing equipment 3 of the second preferred embodiment of the present invention. In FIG. 6, some components and devices are shown in a cross-sectional view.

如圖6所示,與根據本發明之第一較佳具體實施例之製造設備3相同,根據本發明之第二較佳具體實施例之製造設備3同樣包含爐體30、冷卻夾套32以及至少一沉積基板34。不同地,根據本發明之第二較佳具體實施例之製造設備3同樣包含鈍態氣體供應裝置39,而未包含真空抽氣裝置36。鈍態氣體供應裝置39係與冷卻夾套32之第二頂部322連通。圖6中具有與圖3中相同號碼標記之元件、構件、裝置,有相同或類似的結構以及功能,在此不多做贅述。 As shown in FIG. 6, similar to the manufacturing equipment 3 according to the first preferred embodiment of the present invention, the manufacturing equipment 3 according to the second preferred embodiment of the present invention also includes a furnace body 30, a cooling jacket 32, and At least one deposition substrate 34. Differently, the manufacturing equipment 3 according to the second preferred embodiment of the present invention also includes a passive gas supply device 39, but does not include a vacuum pumping device 36. The passive gas supply device 39 is in communication with the second top portion 322 of the cooling jacket 32. Elements, components, and devices in FIG. 6 that have the same reference numerals as those in FIG. 3 have the same or similar structures and functions, and will not be repeated here.

請再參閱圖6及圖7、圖8,利用根據本發明之第二較佳具體實施例之製造設備3製造一氧化矽沉積物46如下文所述。 Please refer to FIG. 6, FIG. 7 and FIG. 8 again, and use the manufacturing equipment 3 according to the second preferred embodiment of the present invention to manufacture the silicon oxide deposit 46 as described below.

如圖6所示,首先,複數顆矽粉體40係置於坩堝5內,再將盛裝複數顆第一矽粉體40的坩堝5置於爐體30內,至少一加熱器306圍繞在坩堝5的外壁。於一具體實施例中,坩堝5可以由石墨所製成,但並不以此為限。 As shown in FIG. 6, first, a plurality of silicon powder bodies 40 are placed in the crucible 5, and then the crucible 5 containing the plurality of first silicon powder bodies 40 is placed in the furnace body 30, and at least one heater 306 surrounds the crucible. 5 outer walls. In a specific embodiment, the crucible 5 may be made of graphite, but is not limited thereto.

如圖7所示,接著,爐體30將複數顆第一矽粉體40加熱至第一溫度且維持一加熱時間,致使每一顆第一矽粉體40表面形成二氧化矽層。多顆矽粉體40變成多顆二氧化矽殼/矽核複合粉體42。第一溫度之範圍以及多顆二氧化矽 殼/矽核複合粉體之Si/SO2比例範圍如上文所述,在此不再贅述。 As shown in FIG. 7, the furnace body 30 heats the plurality of first silicon powder bodies 40 to a first temperature for a heating time, so that a silicon dioxide layer is formed on the surface of each of the first silicon powder bodies 40. The plurality of silicon powders 40 become a plurality of silicon dioxide shell / silicon core composite powders 42. The range of the first temperature and the range of the Si / SO 2 ratio of the plurality of silicon dioxide shell / silicon core powders are as described above, and are not repeated here.

如圖8所示,接著,鈍態氣體供應裝置39接著持續運作供應鈍態氣體(例如,氬氣等)將爐體30內以及冷卻夾套32內形成鈍態氣氛。爐體30接著將多顆二氧化矽殼/矽核複合粉體42或將多顆二氧化矽殼/矽核複合粉體42與新添加的複數顆第二矽粉體(未繪示於圖中)一起加熱至第二溫度,致使每一顆二氧化矽殼/矽核複合粉體42的二氧化矽殼與矽核或每一顆二氧化矽殼/矽核複合粉體42的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一氧化矽蒸氣44。一氧化矽蒸氣44經過通孔300,流入冷卻夾套32內。通孔300還可以避免二氧化矽殼/矽核複合粉體42飛濺進入冷卻夾套32內。 As shown in FIG. 8, the passive gas supply device 39 continues to operate to supply a passive gas (for example, argon) to form a passive atmosphere in the furnace body 30 and the cooling jacket 32. The furnace body 30 then combines a plurality of silicon dioxide shells / silicon core composite powders 42 or a plurality of silicon dioxide shells / silicon core composite powders 42 and a plurality of newly added second silicon powders (not shown in the figure). Middle) together to the second temperature, causing the silica dioxide of each silica shell / silicon core composite powder 42 and the silica or the silica of each silica shell / silicon core composite powder 42 The silicon shell reacts with the silicon core and each second silicon powder to form silicon oxide and sublimate into silicon oxide vapor 44. Silicon monoxide vapor 44 flows through the through hole 300 and flows into the cooling jacket 32. The through hole 300 can also prevent the silicon dioxide shell / silicon core composite powder 42 from splashing into the cooling jacket 32.

冷卻液體L持續從冷卻夾套32之液體入口326流入冷卻夾套32之儲液腔324從冷卻夾套32之液體出口328流出,讓至少一沉積基板34之溫度低於第三溫度,致使流經冷卻夾套32內之一氧化矽蒸氣44沉積於至少一沉積基板34上形成一氧化矽沉積物46。各項製程參數、條件如上文所述,在此不再贅述。圖7及圖8中具有與圖4及圖5中相同號碼標記之元件、構件、裝置,有相同或類似的結構以及功能,在此不多做贅述。 The cooling liquid L continuously flows from the liquid inlet 326 of the cooling jacket 32 into the liquid storage cavity 324 of the cooling jacket 32 and flows out of the liquid outlet 328 of the cooling jacket 32, so that the temperature of at least one deposition substrate 34 is lower than the third temperature, causing A silicon oxide vapor 44 in the cooling jacket 32 is deposited on at least one deposition substrate 34 to form a silicon oxide deposit 46. Various process parameters and conditions are as described above, and will not be repeated here. The components, components, and devices in FIG. 7 and FIG. 8 that have the same reference numerals as those in FIG. 4 and FIG. 5 have the same or similar structures and functions, and will not be repeated here.

進一步,同樣地,根據本發明之第一較佳具體之實施例之製造設備3還包含第一檔板37以及第二檔板38。鈍態氣體供應裝置39係以導管362與冷卻夾套32之第二頂部322連通。第二檔板38係安置於冷卻夾套32內靠近導管362以阻擋一氧化矽蒸氣46進入導管362中。 Further, similarly, the manufacturing apparatus 3 according to the first preferred embodiment of the present invention further includes a first baffle plate 37 and a second baffle plate 38. The passive gas supply device 39 is in communication with the second top portion 322 of the cooling jacket 32 through a conduit 362. The second baffle plate 38 is disposed in the cooling jacket 32 near the duct 362 to block the silicon oxide vapor 46 from entering the duct 362.

與先前技術相比較,本發明所採用的二氧化矽殼/矽核複合粉體,二氧化矽與矽接觸的面積較大。因此,執行 本發明之方法的製造設備,其整體體積較小,且較不耗能,單位時間內的產能較高。 Compared with the prior art, the silicon dioxide shell / silicon core composite powder used in the present invention has a larger contact area between silicon dioxide and silicon. So execute The manufacturing equipment of the method of the present invention has a small overall volume, consumes less energy, and has a higher capacity per unit time.

藉由以上較佳具體實施例之詳述,係希望能更加清楚描述本發明之特徵與精神,而並非以上述所揭露的較佳具體實施例來對本發明之面向加以限制。相反地,其目的是希望能涵蓋各種改變及具相等性的安排於本發明所欲申請之專利範圍的面向內。因此,本發明所申請之專利範圍的面向應該根據上述的說明作最寬廣的解釋,以致使其涵蓋所有可能的改變以及具相等性的安排。 With the above detailed description of the preferred embodiments, it is hoped that the features and spirit of the present invention may be more clearly described, rather than limiting the aspects of the present invention with the preferred embodiments disclosed above. On the contrary, the intention is to cover various changes and equivalent arrangements within the scope of the patent scope of the present invention. Therefore, the aspect of the patent scope of the present invention should be explained in the broadest sense according to the above description, so that it covers all possible changes and equal arrangements.

Claims (15)

一種製造一一氧化矽沉積物之方法,包含下列步驟:製備複數顆矽粉體;將該複數顆矽粉體加熱至一第一溫度且維持一加熱時間,致使每一顆矽粉體表面形成一二氧化矽層,該多顆矽粉體變成複數顆二氧化矽殼/矽核複合粉體;將該複數顆二氧化矽殼/矽核複合粉體置於一真空環境或一鈍態氣氛中且加熱至一第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核反應成一氧化矽且昇華成一一氧化矽蒸氣;以及收集且冷卻該一氧化矽蒸氣,即獲得該一氧化矽沉積物。A method for manufacturing a silicon oxide deposit includes the following steps: preparing a plurality of silicon powders; heating the plurality of silicon powders to a first temperature and maintaining a heating time, so that the surface of each silicon powder is formed A silicon dioxide layer, the plurality of silicon powders are changed into a plurality of silicon dioxide shells / silicon core composite powders; the plurality of silicon dioxide shells / silicon core composite powders are placed in a vacuum environment or a passive state Medium and heated to a second temperature, causing the silica shell of each silica shell / silicon core composite powder to react with the silica core to form silicon oxide and sublimate into a silicon oxide vapor; and collect and cool the oxide Silicon vapor, the silicon monoxide deposit is obtained. 如請求項1所述之方法,其中該複數顆二氧化矽殼/矽核複合粉體之一整體密度範圍為從0.62g/cm3至0.68g/cm3,該複數顆二氧化矽殼/矽核複合粉體之一Si/SO2莫耳數比例範圍為從0.8至1.2。The method according to claim 1, wherein one of the plurality of silica dioxide shells / silicon core composite powders has an overall density ranging from 0.62 g / cm 3 to 0.68 g / cm 3 , and the plurality of silica shells / One of the silicon core composite powders has a Si / SO 2 mole ratio ranging from 0.8 to 1.2. 如請求項2所述之方法,其中該第一溫度之範圍為從600℃至900℃,該第二溫度之範圍為從1200℃至1450℃。The method according to claim 2, wherein the first temperature ranges from 600 ° C to 900 ° C, and the second temperature ranges from 1200 ° C to 1450 ° C. 一種製造一一氧化矽沉積物之方法,包含下列步驟:製備複數顆第一矽粉體;將該複數顆第一矽粉體加熱至一第一溫度且維持一加熱時間,致使每一顆第一矽粉體表面形成一二氧化矽層,該複數顆第一矽粉體變成複數顆二氧化矽殼/矽核複合粉體;將該複數顆二氧化矽殼/矽核複合粉體與複數第二矽粉體置於一真空環境或一鈍態氣氛中且加熱至一第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一一氧化矽蒸氣;以及收集且冷卻該一氧化矽蒸氣,即獲得該一氧化矽沉積物。A method for manufacturing a silicon oxide deposit includes the following steps: preparing a plurality of first silicon powders; heating the plurality of first silicon powders to a first temperature and maintaining a heating time, so that each A silicon dioxide layer is formed on the surface of a silicon powder, and the plurality of first silicon powders become a plurality of silicon dioxide shells / silicon core composite powders; the plurality of silicon dioxide shells / silicon core composite powders and a plurality of The second silicon powder is placed in a vacuum environment or a passive atmosphere and heated to a second temperature, so that the silicon dioxide shell and silicon core of each silicon dioxide shell / silicon core composite powder and each The second silicon powder is reacted into silicon monoxide and sublimates into silicon monoxide vapor; and the silicon monoxide vapor is collected and cooled to obtain the silicon monoxide deposit. 如請求項4所述之方法,其中該第一溫度之範圍為從600℃至900℃,該第二溫度之範圍為從1200℃至1450℃。The method according to claim 4, wherein the first temperature ranges from 600 ° C to 900 ° C, and the second temperature ranges from 1200 ° C to 1450 ° C. 一種製造設備,包含:一爐體,其中複數顆第一矽粉體係置於該爐體內;一冷卻夾套,係安置於該爐體之一第一頂部上且與該爐體之該第一頂部連通,該冷卻夾套具有一儲液腔、一液體入口以及一液體出口;至少一沉積基板,係放置於該冷卻夾套內且與該冷卻夾套之一內壁熱耦合;以及一真空抽氣裝置,係與該冷卻夾套之一第二頂部連通;其中該爐體將該複數顆第一矽粉體加熱至一第一溫度且維持一加熱時間,致使每一顆第一矽粉體表面形成一二氧化矽層,該複數顆第一矽粉體變成複數顆二氧化矽殼/矽核複合粉體;該真空抽氣裝置接著持續運作將該爐體內以及該冷卻夾套內形成一真空環境;該爐體接著將該複數顆二氧化矽殼/矽核複合粉體或將該複數顆二氧化矽殼/矽核複合粉體與新添加的複數顆第二矽粉體一起加熱至一第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核反應或每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一一氧化矽蒸氣;一冷卻液體從該液體入口流入該儲液腔從該液體出口流出,讓該至少一沉積基板之溫度低於一第三溫度,致使流經該冷卻夾套內之該一氧化矽蒸氣沉積於該至少一沉積基板上形成一一氧化矽沉積物。A manufacturing equipment includes: a furnace body, in which a plurality of first silicon powder systems are placed in the furnace body; and a cooling jacket, which is arranged on a first top of one of the furnace bodies and is connected to the first of the furnace body. The cooling jacket has a liquid storage cavity, a liquid inlet, and a liquid outlet; at least one deposition substrate is placed in the cooling jacket and is thermally coupled to an inner wall of the cooling jacket; and a vacuum The air extraction device is in communication with a second top of the cooling jacket; wherein the furnace body heats the plurality of first silicon powder bodies to a first temperature and maintains a heating time, so that each of the first silicon powder bodies A silicon dioxide layer is formed on the surface of the body, and the plurality of first silicon powders are changed into a plurality of silicon dioxide shell / silicon core composite powders; the vacuum extraction device continues to operate to form the furnace body and the cooling jacket. A vacuum environment; the furnace body then heats the plurality of silica dioxide shells / silicon core composite powders or the plurality of silica dioxide shells / silicon core composite powders with the newly added plurality of second silica powders To a second temperature, causing every dioxin The silica shell of the silicon shell / silicon core composite powder reacts with the silicon core or the silicon dioxide shell of each silicon dioxide shell / silicon core composite powder reacts with the silicon core and each second silicon powder to form an oxide Silicon and sublimates into silicon monoxide vapor; a cooling liquid flows from the liquid inlet into the liquid storage cavity and flows out from the liquid outlet, so that the temperature of the at least one deposition substrate is lower than a third temperature, causing it to flow through the cooling jacket The silicon oxide vapor is deposited on the at least one deposition substrate to form a silicon oxide deposit. 如請求項6所述之製造設備,進一步包含一第一檔板,係安置於該至少一沉積基板所圍成之一空間之一上方,其中該一氧化矽蒸氣也沉積於該第一檔板上。The manufacturing equipment according to claim 6, further comprising a first baffle plate, which is disposed above one of a space surrounded by the at least one deposition substrate, wherein the silicon monoxide vapor is also deposited on the first baffle plate. on. 如請求項7所述之製造設備,進一步包含一第二檔板,其中該真空抽氣裝置係以一導管與該冷卻夾套之該第二頂部連通,該第二檔板係安置於該冷卻夾套內靠近該導管以阻擋該一氧化矽蒸氣被抽出該冷卻夾套。The manufacturing equipment according to claim 7, further comprising a second baffle, wherein the vacuum pumping device is connected to the second top of the cooling jacket by a duct, and the second baffle is disposed on the cooling The jacket is close to the conduit to prevent the silicon monoxide vapor from being drawn out of the cooling jacket. 如請求項8所述之製造設備,其中該複數顆二氧化矽殼/矽核複合粉體之一整體密度範圍為從0.62g/cm3至0.68g/cm3,該複數顆二氧化矽殼/矽核複合粉體之一Si/SO2莫耳數比例範圍為從0.8至1.2。The manufacturing equipment according to claim 8, wherein one of the plurality of silica dioxide shells / silicon core composite powders has an overall density ranging from 0.62 g / cm 3 to 0.68 g / cm 3 , the plurality of silica shells The Si / SO 2 molar ratio of one of the silicon / silicon core composite powders ranges from 0.8 to 1.2. 如請求項9所述之製造設備,其中該第一溫度之範圍為從600℃至900℃,該第二溫度之範圍為從1200℃至1450℃,該第三溫度為400℃。The manufacturing equipment according to claim 9, wherein the first temperature range is from 600 ° C to 900 ° C, the second temperature range is from 1200 ° C to 1450 ° C, and the third temperature is 400 ° C. 一種製造設備,包含:一爐體,其中複數顆第一矽粉體係置於該爐體內;一冷卻夾套,係安置於該爐體之一第一頂部上且與該爐體之該第一頂部連通,該冷卻夾套具有一儲液腔、一液體入口以及一液體出口;至少一沉積基板,係放置於該冷卻夾套內且與該冷卻夾套之一內壁熱耦合;以及一鈍態氣體供應裝置,係與該冷卻夾套之一第二頂部連通;其中該爐體將該複數顆第一矽粉體加熱至一第一溫度且維持一加熱時間,致使每一顆第一矽粉體表面形成一二氧化矽層,該複數顆第一矽粉體變成複數顆二氧化矽殼/矽核複合粉體;該鈍態氣體供應裝置接著持續運作供應一鈍態氣體將該爐體內以及該冷卻夾套內形成一鈍態氣氛;該爐體接著將該複數顆二氧化矽殼/矽核複合粉體或將該複數顆二氧化矽殼/矽核複合粉體與新添加的複數顆第二矽粉體一起加熱至一第二溫度,致使每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核反應或每一顆二氧化矽殼/矽核複合粉體的二氧化矽殼與矽核以及每一顆第二矽粉體反應成一氧化矽且昇華成一一氧化矽蒸氣;一冷卻液體從該液體入口流入該儲液腔從該液體出口流出,讓該至少一沉積基板之溫度低於一第三溫度,致使流經該冷卻夾套內之該一氧化矽蒸氣沉積於該至少一沉積基板上形成一一氧化矽沉積物。A manufacturing equipment includes: a furnace body, in which a plurality of first silicon powder systems are placed in the furnace body; and a cooling jacket, which is arranged on a first top of one of the furnace bodies and is connected to the first of the furnace body. The cooling jacket is connected at the top, and the cooling jacket has a liquid storage cavity, a liquid inlet and a liquid outlet; at least one deposition substrate is placed in the cooling jacket and is thermally coupled to an inner wall of the cooling jacket; and a blunt Gas supply device is in communication with a second top of one of the cooling jackets; wherein the furnace body heats the plurality of first silicon powders to a first temperature and maintains a heating time, so that each of the first silicon powders A silicon dioxide layer is formed on the surface of the powder, and the plurality of first silicon powders become a plurality of silicon dioxide shell / silicon core composite powders. The passive gas supply device then continuously operates to supply a passive gas to the furnace body. And a passive atmosphere is formed in the cooling jacket; the furnace body then combines the plurality of silicon dioxide shells / silicon core composite powders or the plurality of silicon dioxide shells / silicon core composite powders with the newly added plurality The second silicon powder is heated to the first The temperature causes the silicon dioxide shell of each silicon dioxide shell / silicon core composite powder to react with the silicon core or the silicon dioxide shell and silicon core of each silicon dioxide shell / silicon core composite powder and each The second silicon powder reacts into silicon oxide and sublimates into silicon monoxide vapor; a cooling liquid flows from the liquid inlet into the liquid storage cavity and flows out from the liquid outlet, so that the temperature of the at least one deposition substrate is lower than a third temperature Causing the silicon oxide vapor flowing through the cooling jacket to be deposited on the at least one deposition substrate to form a silicon oxide deposit. 如請求項11所述之製造設備,進一步包含一第一檔板,係安置於該至少一沉積基板所圍成之一空間之一上方,其中該一氧化矽蒸氣也沉積於該第一檔板上。The manufacturing equipment according to claim 11, further comprising a first baffle plate, which is disposed above one of a space surrounded by the at least one deposition substrate, wherein the silicon monoxide vapor is also deposited on the first baffle plate. on. 如請求項12所述之製造設備,進一步包含一第二檔板,其中該鈍態氣體供應裝置係以一導管與該冷卻夾套之該第二頂部連通,該第二檔板係安置於該冷卻夾套內靠近該導管以阻擋該一氧化矽蒸氣進入該導管中。The manufacturing equipment according to claim 12, further comprising a second baffle, wherein the passive gas supply device is connected to the second top of the cooling jacket by a duct, and the second baffle is disposed on the The cooling jacket is close to the conduit to block the silicon monoxide vapor from entering the conduit. 如請求項13所述之製造設備,其中該複數顆二氧化矽殼/矽核複合粉體之一整體密度範圍為從0.62g/cm3至0.68g/cm3,該複數顆二氧化矽殼/矽核複合粉體之一Si/SO2莫耳數比例範圍為從0.8至1.2。The manufacturing equipment according to claim 13, wherein one of the plurality of silica dioxide shells / silicon core composite powders has an overall density ranging from 0.62 g / cm 3 to 0.68 g / cm 3 , the plurality of silica shells The Si / SO 2 molar ratio of one of the silicon / silicon core composite powders ranges from 0.8 to 1.2. 如請求項14所述之製造設備,其中該第一溫度之範圍為從600℃至900℃,該第二溫度之範圍為從1200℃至1450℃,該第三溫度為400℃。The manufacturing equipment according to claim 14, wherein the first temperature ranges from 600 ° C to 900 ° C, the second temperature ranges from 1200 ° C to 1450 ° C, and the third temperature is 400 ° C.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5096685A (en) * 1985-07-27 1992-03-17 Kawasaki Steel Corporation Method for manufacturing fine-grained silicon monoxide
CN101010444A (en) * 2004-09-01 2007-08-01 住友钛株式会社 SiO deposition material, raw material si powder, and method for producing siO deposition material
JP2017202945A (en) * 2016-05-09 2017-11-16 信越化学工業株式会社 Apparatus and method for producing silicon monoxide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5096685A (en) * 1985-07-27 1992-03-17 Kawasaki Steel Corporation Method for manufacturing fine-grained silicon monoxide
CN101010444A (en) * 2004-09-01 2007-08-01 住友钛株式会社 SiO deposition material, raw material si powder, and method for producing siO deposition material
JP2017202945A (en) * 2016-05-09 2017-11-16 信越化学工業株式会社 Apparatus and method for producing silicon monoxide

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