TW200418723A - Involved fullerene manufacturing and collecting system tool - Google Patents

Involved fullerene manufacturing and collecting system tool Download PDF

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Publication number
TW200418723A
TW200418723A TW092135886A TW92135886A TW200418723A TW 200418723 A TW200418723 A TW 200418723A TW 092135886 A TW092135886 A TW 092135886A TW 92135886 A TW92135886 A TW 92135886A TW 200418723 A TW200418723 A TW 200418723A
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Taiwan
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substrate
solution
chamber
fullerene
dissolving
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TW092135886A
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Chinese (zh)
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Rikizo Hatakeyama
Kenji Omote
Yasuhiko Kasama
Takamichi Hirata
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Ideal Star Inc
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/152Fullerenes
    • C01B32/156After-treatment

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Composite Materials (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

This invention provides a fullerene manufacturing and collecting system tool capable of manufacturing a high quality involved fullerene with a high production efficiency, comprising a vacuum chamber (1), a film formation chamber (5) having a substrate inlet port (2a) for leading a substrate (3a) therein formed on the vacuum chamber (1) side and stacking the involved fullerene on the substrate (2a), a dissolving chamber (6) having a substrate inlet port (2b) for leading, therein, a substrate (3b) on which the involved fullerene was stacked in the film formation chamber (5) formed on the vacuum chamber (1) side and also having a dissolving liquid inlet port (9) for leading dissolving liquid for melting the involved fullerene stacked on the substrate (2b) and a dissolving liquid outlet port (10) for discharging the dissolving liquid (this dissolving liquid is referred to as "resolvent") after the involved fullerene is dissolved, and susceptors (4a, 4b) allowed to be rotated and reciprocatingly moved, allowing a plurality of substrates to be placed thereon, and capable of leading the substrates into the film formation chamber (5) and the dissolving chamber (6).

Description

200418723 五、發明說明(l) 本發明係關於一種内包富勒烯的製造 【發明所屬之技術領域 【先前技術】 在西元1 9 9 0年,由Kratshmer (人名)發表C6〇所代表 之管狀且中空之碳叢集、所謂富勒稀之大量合成法 (W. K r a t s hmer et al·,Nature (人名),347 (199〇) 3 54 )。向來,這個本身係本來就進行C6〇結晶之各種物 研究。200418723 V. Description of the invention (l) The present invention relates to the manufacture of a fullerene encased [Technical field to which the invention belongs [prior art] In 1990, Kratshmer (person name) published a tubular and Hollow carbon clusters, the so-called fullerene mass synthesis method (W. K rats hmer et al., Nature (person name), 347 (199〇) 3 54). This has always been the study of various C6O crystals.

此外,运報告藉由Hebard (人名)們之所造 在C60薄膜摻雜K之K3C60來顯示臨界溫度^^“之超^ 之報告(A.F.Hebard et al m Q, . (1990 6 0 0 )。這個係著/点= tUre (人名),350 夕户而 ,?目士 ’、者眼成為新的超傳導體材料。 率來得到内包富勒烯之方 :確立在基板上、以高良ίIn addition, this report uses K3C60 doped with K in C60 thin films made by Hebard (person names) to show the critical temperature ^^ "exceeding ^ (AFHebard et al m Q,. (1990 6 0 0). This tie / point = tUre (person's name), 350, and the “eyes” and “eyes” become the new superconductor material. The rate to get the fullerene side: established on the substrate, with high quality.

在裝置内壁或基板上之所^二也就是說,在現在時間點, 極為少量。 于到之内包富勒烯量係僅不過J 在目前現狀,隨荖# _ I , 或基板上之所得到之内包^ 無法確立回收在裝置户That is, on the inner wall of the device or on the substrate, that is, at the present point in time, it is extremely small. The amount of fullerene included in the package is only the current status of J. With the # _ I, or the package obtained on the substrate ^ Cannot establish recycling in the device user

藉由任何_冑方法而:::之方&。例如實際狀I (内包富勒烯)。更何;;θ回收附著在裝置内壁上之难 高回收率地回收内包舍勒=以工業水準、生產效率良女 言,也成為完全二=法係即使是對於研以 相對於此,本發明人係另外提供以高良品率而得至By any of the methods ::: 之 方 &. For example, the actual state I (fullerene inclusive). What's more; θ recovery is difficult to recover attached to the inner wall of the device. High recovery rate. Inner package Scholler = industrial level and good production efficiency. It also becomes a complete second = law system. Even for the research, the present invention Human department additionally provides with high yield

200418723 五、發明說明(2) — ,之内包J勒烯之技術(曰本特願2〇〇 内包富勒歸而確立 内 。要求對於 收率且生產效率_样祕、# y义Η匕田勒%之特性、以丄A 本發 旱良好地進行回收之技術。 M鬲回 士月之目的係提供_種 率地來製造及回收高品質 ,良好且高生 造•回收系統工具。 勒烯之内包富勒烯的制 【發明内容] & 本發明之内包富勒稀 fr括:真空室;在該真;;側具,其特徵 成膜室;在該成膜室、二:包富勒婦之堆積; 包富勒稀堆積之基板之基板導二以導入進行内 行堆積在基板上之内包舍 並且具有用以導入來進 液導入口以及用以排出:溶解:Τ:之溶解用液之溶解用 (將該溶解用液稱為「溶t内匕昌勒烯後之溶解用液 室;以及能夠進行旋轉及往=動=溶解液排出口的溶解 板而能夠將基板導入至 ,作並且可以載置複數個基 W述内包6/ 戰态。 二 田勒烯係金屬内包富勒。 ‘ i屬係鹼金屬。 成為内包狀態之富勒烯。2用液係笨胺。苯胺係不溶解不 因此,可以藉由使得笨三苯胺係溶解内包富勒烯。 結果,能夠回收並非成古為溶媒而僅回收内包富勒烯。 苯胺係可以適合使用作^ =回收率方面之富勒烯。此外, 為馬速色譜法(HPLC)之展開液。 其特徵在於 其特徵在於 其特徵在於:前述內~、;!;或該溶解室的承載器 200418723 五 、發明說明(3) 其特徵在於:形成:在某一端 入口之導入通路以月/京一俨且古、有用以導入〉谷液之導 ‘排出口之排出通路;纟得該導入通路和 :'、、先外 於各個其他端而形成交差部’同日夺,將呈‘在兮!: J交差 置朝向基板來成為開口狀之開口部所構:之喷;設 及用以控制接觸到基板之溶液壓力和大氣壓體以 過該開口部來使得接觸釗基板之溶 ^而透 外之壓力控制手段…,設置在前述排以 出口和該排出口。 連接則述〉谷解液排 其特徵在於:設置用以賦予超音波至該溶解液之手 段。可以藉由賦予超音波而使得由基板容易脫離堆積在美 板之内包富勒烯,以便於更加地提高内包富勒烯之回收土 率〇 ^ /、〜心%汉> ^ τ欣而退打丞 板之洗淨。也就是說,如果是在溶解作業後而切換閥來導 也可以進行基板之洗淨。當然,也可以 其特欲在於··在前述洛解用液導入口之下游,設置切 換閥\切換閥之某一邊係連接在溶解用液,其他邊=連接 在洗淨液。為了進行基板之洗淨,因此,正如前面敘述, 可以設置洗淨室,但是,即使是不刻意地設置洗淨室,也 可以藉由在溶解用液導入口之下游,設置切換閥,切換閥 之某一邊連接在溶解用液,其他邊連接在洗淨液而進行基 之洗淨。也就是說,如果是在溶解作業德 入洗淨液的話,則一 ^ ^ 一起進行此種洗淨和洗淨室之洗淨。 其特彳政在於··在$述成膜室和前述溶解室間,設置用200418723 V. Description of the invention (2) —, the technology of enclosing J lerene (this version is specially established to enclose the fuller in 2000. It is required that the yield and production efficiency _ 样 秘 、 # y 义 Η 刀 田The characteristics of Le%, and the technology of good recovery with the drought of 丄 A. The purpose of M 鬲 Shishiyue is to provide _species to manufacture and recycle high-quality, good and high-quality production and recycling system tools. Production of Inner Fullerene [Summary of the Invention] & Inner Fullerene in the present invention includes: vacuum chamber; in the true ;; side with its characteristic film forming chamber; in the film forming chamber, two: fuller The substrates of the substrates that cover the Fuller ’s thinly stacked substrates are stacked in-line on the substrate and are provided with an inlet for liquid introduction and a discharge solution for dissolution: dissolution: T: For dissolution (this solution for dissolution is referred to as "the dissolution liquid chamber after dissolving the changlerene; and the dissolving plate capable of rotating and moving = moving = dissolving liquid discharge port, the substrate can be introduced to, and Multiple bases can be placed to describe the inclusive 6 / state of war. Fullerene is enclosed in metal. 'I is a type of alkali metal. Fullerene in an enclosed state. 2 Liquid benzylamine is used. Aniline is insoluble. Therefore, the fullerene can be dissolved by dissolving benzyltriphenylamine. As a result, It can recover not only the fullerenes but also the fullerenes. The aniline system can be used as a fullerene in the recovery rate. In addition, it is a developing solution for horse speed chromatography (HPLC). It is characterized by its characteristics It is characterized by the following: ~~;!; Or the carrier of the dissolution chamber 200418723 V. Description of the invention (3) It is characterized by the formation: the entrance path at the entrance of a certain end is ancient and useful. "Introduction> Guide of liquid guide" the discharge path of the discharge port; I won the introduction path and: ", first formed at the other end of the intersection with the intersection" on the same day, will be "in the Xi !: J intersection is placed towards the substrate To be an opening-shaped opening portion: a spray; a pressure control means for controlling the pressure of the solution contacting the substrate and the atmospheric pressure body to pass through the opening portion to make the contact with the substrate ^… in The discharge port is connected with the discharge port. The connection solution> Gujie liquid discharge port is characterized in that it is provided with a means for imparting ultrasound to the dissolving solution. The substrate can be easily separated from and deposited on the US board by giving an ultrasonic wave. Fullerene is enclosed in order to further increase the recovery soil rate of enclosed fullerenes. ^ /, ~ %% han > ^ τ, and wash back the hiccups. In other words, if it is in the dissolving operation Later, the switching valve can also be used to clean the substrate. Of course, it can also be special ..... downstream of the above-mentioned solution introduction inlet, one side of the switching valve \ switching valve is connected to the dissolution liquid. The other side = connected to the cleaning solution. In order to clean the substrate, as described above, a cleaning chamber can be installed, but even if the cleaning chamber is not intentionally set, it can be introduced by the solution for dissolution. A switching valve is installed downstream of the mouth. One side of the switching valve is connected to the dissolving liquid, and the other side is connected to the washing liquid to perform basic cleaning. In other words, if the cleaning solution is used in the dissolution operation, the cleaning and the cleaning of the cleaning room are performed together. Its special policy is to install a space between the film formation chamber and the dissolution chamber.

2015-6047-PF(Nl).ptd 第8頁 200418723 五、發明說明(4) f 芩 將; 内、導入洗淨液而進行洗淨的話喷=體設置在洗淨室 淨。 則也可以簡單地進行洗 甘、特诫在於··在前述溶解室,連接 ,、特徵在於··在前述柱 / ,之色譜法用;^主。 其特徵在於:前述柱及連接成分分析機器。 空室内。 及則述成分分析機器係配置在真 【實施方式】 (實施例1 ) 工具在圖丨’顯示本例子之内包富勒稀的製造·回收系統 = :2a並且用m行對於基板3a上之内之基板導 舍iV *成膜室5、於真空室1側具有用:導入進堆積內之成 田勒細堆積之基板3b之基板導入 導入進仃内包 進行堆積在基板2b上之内包富勒烯、,容解^;; 以導入來 解用液導入口 9以及用以排解/液之溶 用液(將該溶解用液稱為「溶解液」)之田溶勒^夜後之溶解 之溶解室6 ;以及能夠進行旋轉及往復動 卜出口101 複數個基板而能夠將基板導入至 i =以載置 載器4a、4b。 _至5或^解室6之承 根據圖1而更加詳細地說明本例子。 第9頁 2015-6047-PF(Nl).ptd 200418723 五、發明說明(5) 在真空室1,設置成膜室5和溶解室6。成膜室5係在真 空室1側,具有開口部。該開口部係成為用以導入基板3 a 之基板導入口 2a。 此外,在本例子,鄰接於真空室1而設置閘閥11。為 了進行富勒烯之堆積,因此,在基本上,並不需要進行基 板之交換。也就是說,可以重複地使用基板。只是,也可 以透過閘閥1 1而將新的基板,導入至真空室。 在成膜室5,進行内包富勒稀之堆積。如果能夠進行 内包富勒烯之堆積的話,則成膜室5之内部構造係並無特 別限定。 φ 另一方面,溶解室6係在真空室1側,設置用以導入呈 開口狀之基板3b之基板導入口 2b。在溶解室2,形成溶解 用溶液導入口 9以及溶解液排出口 1 0。由溶解用溶液導入 口 9而導入用以溶解内包富勒烯之溶解用溶液(溶媒)。 内包富勒烯溶解後之溶解液係由溶解液排出口 9而排出至 溶解室6之外部。溶解液排出口 9係可以設置在溶解室之下 面,藉由重力而排出溶解液。或者是藉由吸引而進行排 出。 藉由在溶解液排出口 9之下游,設置例如溶液色譜法 (特別是高速溶液色譜法)用柱而進行内包富勒烯之分離❿ •精製。可以在柱之下游,設置用以分析内包富勒烯成分 等之分析裝置。可以將來自分析裝置之訊號,傳送至成膜 室5而控制成膜條件。 此外,可以在真空室内,設置用以乾燥内包富勒烯或2015-6047-PF (Nl) .ptd Page 8 200418723 V. Description of the invention (4) f 芩 If the inside and inside are cleaned by introducing the washing liquid, the spray body is set in the washing room. It can also be simply washed, and the special command is that: in the aforementioned dissolution chamber, the connection is characterized by the use of chromatography in the aforementioned column /, the main method. It is characterized by the aforementioned column and connecting component analysis machine. Empty interior. The component analysis machine is arranged in the real [Embodiment] (Example 1) The tool is shown in the figure 丨 'This example includes Fullerene's manufacturing and recycling system =: 2a and uses m rows for the substrate 3a The substrate guide iV * film forming chamber 5 is provided on the side of the vacuum chamber 1 for the introduction of the substrate 3b of Narita Le finely deposited substrate into the stack, the introduction of the substrate into the inner package to deposit fullerene on the substrate 2b, The solution is introduced into the solution introduction port 9 and the solution solution used to dissolve / dissolve the solution (this solution is called "dissolution solution"). 6; and a plurality of substrates can be rotated and reciprocated, and the substrates can be introduced to i = to place the carriers 4a, 4b. The inheritance of _ to 5 or ^ solution room 6 will be described in more detail with reference to FIG. 1. Page 9 2015-6047-PF (Nl) .ptd 200418723 V. Description of the invention (5) In the vacuum chamber 1, a film forming chamber 5 and a dissolution chamber 6 are provided. The film forming chamber 5 is provided on the vacuum chamber 1 side and has an opening. This opening is a substrate introduction port 2a for introducing the substrate 3a. In this example, a gate valve 11 is provided adjacent to the vacuum chamber 1. In order to carry out the accumulation of fullerenes, it is basically not necessary to exchange substrates. That is, the substrate can be reused. However, a new substrate may be introduced into the vacuum chamber through the gate valve 11. In the film formation chamber 5, accumulation of fullerene is carried out. The internal structure of the film forming chamber 5 is not particularly limited as long as the fullerene-inclusive deposition can be performed. φ On the other hand, the dissolution chamber 6 is provided on the vacuum chamber 1 side, and a substrate introduction port 2b for introducing an opening-shaped substrate 3b is provided. In the dissolution chamber 2, a dissolution solution introduction port 9 and a dissolution solution discharge port 10 are formed. From the dissolution solution introduction port 9, a dissolution solution (solvent) for dissolving the fullerene incorporation is introduced. The dissolved solution containing the fullerene dissolved therein is discharged to the outside of the dissolution chamber 6 through the dissolution solution discharge port 9. Dissolving solution discharge port 9 can be installed under the dissolution chamber to discharge the dissolving solution by gravity. Or discharge by attraction. A fullerene-encapsulated separation is performed by installing a column for solution chromatography (especially high-speed solution chromatography) downstream of the dissolving solution discharge port 9 • Purification. An analysis device may be provided downstream of the column for analyzing the fullerene content and the like. The signal from the analysis device can be transmitted to the film forming chamber 5 to control the film forming conditions. In addition, it can be installed in a vacuum chamber to dry the fullerene or

2015-6047-PF(Nl).ptd 第10頁 200418723 五、發明說明(6) 基板之乾燥室 在該狀2下最ί f將柱、分析機器,配置在真空室1内。 空室1内。可=士室6之溶解液排出口10係設置位處在直 由成膜至分析Λ 樣構成而不接觸到大氣,來進行 接著:=,可以得到更高品質之内包富勒稀。仃 # 就承載器而進行說明。 ^ 以載内/設置能夠進行旋轉及往復動作並且可 室5或A 土板3a、3b而用以將基板3a、3b導入至点 或洛解室6之配置在真空幻内之承載⑽、#成聪 Π載器係分割成為2個承載器切、“,但是,ίΐ ^為-體。此m也在㈣導人基板至成膜也可 冷解室Θ之位置上,設計及配置承載器。 、至 在圖1所示之例子,於承載器4a、4b上分 Γ在Vb。此外,例如在真空室側設置開口及配置洗、爭二 而在洗淨室來進行基板洗淨之狀態了,還Μ載g先^ 另夕卜一個基板。也就是說1對應於進行對板U 之處理室數目之數目之基板,載置在承載器。板之處理 承載态4 a、4 b係藉由保持體8而進行保持。 載器4a、4b而載置基板3a、3b之狀態來上升保持體8日士 7, 基板3a、3b係分別透過導入口 2a、2b而導入至成膜. 溶解室6。在分別導入基板3&、3b之狀態下,於成膜\、 溶解室6之底面和承載器4a、札間,形成密封狀能,、=、 室5、溶解室6之内部係成為氣密狀態。當然,為\风膜 高氣密性,因此,可以在承載器4a、“和成膜室5、溶°解2015-6047-PF (Nl) .ptd Page 10 200418723 V. Description of the invention (6) Drying chamber for substrate In this state, the column and analysis machine are arranged in the vacuum chamber 1. Inside the empty room 1. It can be set that the dissolution liquid discharge port 10 of the taxi chamber 6 is directly formed from the film formation to the analysis of the sample without contacting the atmosphere. Then: =, you can get a higher quality fullerene.仃 # Describes the carrier. ^ It can be rotated and reciprocated in the load / set, and can be used to introduce the substrates 3a, 3b to the point 5 or A soil plate 3a, 3b. The Cheng Cong II carrier system is divided into two carriers, ", but, ΐ 为 is -body. This m also designs and configures the carrier at the position where the substrate is guided to the film formation and also the cooling chamber Θ. To the example shown in FIG. 1, Γ is divided into Vb on the carriers 4a and 4b. In addition, for example, a state in which an opening is provided on the vacuum chamber side and washing is arranged, and the substrate is cleaned in the cleaning chamber is washed. In addition, a substrate is also loaded on the substrate. In other words, 1 corresponds to the number of substrates in the processing chamber of the plate U, and is placed on the carrier. The processing load of the plate is 4 a, 4 b. It is held by the holder 8. The carriers 4a and 4b are placed on the substrates 3a and 3b to raise the holder 8 to 7 and the substrates 3a and 3b are introduced into the film through the inlets 2a and 2b, respectively. Dissolution chamber 6. In the state where the substrates 3 & and 3b are respectively introduced, it is formed on the bottom of the film formation chamber, the dissolution chamber 6, and the carrier 4a and the interlayer. The sealing energy can be airtight inside the chamber 5 and the dissolution chamber 6. Of course, it is \ air film with high air tightness, so it can be dissolved in the carrier 4a, "and the film forming chamber 5,

2015-6047-PF(Nl).ptd 第11頁 五 發明說明(7) J6之底面間’設置〇型環圈等。此 ii進:為基板。也就是說…在d:承载器 接地進仃内包富勒烯之堆積。 在承载為之表面,直 之底面及接觸貝到該底面之 Π;:,最好是進行鏡面精加工 為了 任V入基板3a、3b之灿妒π ^ 富勒烯之堆積。在堆積 J,下降成膜室5,進行内包 空室1内係保持在真空或減壓臭狀能 U體8。此時,真 以態。藉由下降保持體δ而;得基板3=上= 成膜室5、溶解室6,來取出至直空Μ ⑼:別由 ^而使得堆積内包富勒烯之基板溶=保持 方。此日寺,基板3b係位處在成膜室5之下方至=至6之下 基板3b導入至成膜室5内,同時/堆// 富勒婦之基板3a,導入至溶解室6 ::將堆積内包 膜室5内,進行内包富勒烯之堆積。同時;:2下’:成 室6内,進行堆積於基板3 内 烯^ ’在溶解 下,重複地進行前述操作。内之溶解。以 像這樣,内包富勒烯係並無曝露在大 以得到高品質之内包富勒烯,同時 因$ :可 溶解而以高生產效率,來製造内包富勒稀。寸進仃成膜和 (實施例2 ) 在圖2 ’顯示實施例2。2015-6047-PF (Nl) .ptd Page 11 V. Description of the invention (7) Between the bottom surface of J6, an O-ring and the like are provided. This step is the substrate. That is to say, the fullerene deposits are packed in the d: carrier grounded. On the surface of the bearing, the bottom surface and the contact surface to the bottom surface are preferably mirror-finished in order to accumulate the full π ^ fullerene accumulation on the substrates 3a and 3b. At stack J, the film-forming chamber 5 is lowered, and the inner envelope 1 is maintained at a vacuum or reduced pressure odorous energy U body 8. At this point, it's true. By lowering the holder δ, the substrate 3 = upper = film-forming chamber 5 and dissolution chamber 6 are taken out to the space M ⑼: Do not make the stacked fullerene-containing substrates dissolved by the ^ = hold side. At this temple, the substrate 3b is located below the film-forming chamber 5 to = to 6. The substrate 3b is introduced into the film-forming chamber 5, and the substrate 3a of the / fuller woman is introduced into the dissolution chamber 6: : Stacking the inner envelope chamber 5 to deposit the fullerene. Simultaneously ;: 2 times': In the forming chamber 6, the substrate 3 is deposited in the substrate 3, and the aforementioned operations are repeated while being dissolved. Dissolve within. In this way, the inner fullerenes are not exposed to obtain high-quality inner fullerenes, and at the same time, the fullerenes are produced with high production efficiency because they are soluble. Inch film formation (Example 2) Example 2 is shown in FIG. 2 '.

200418723 五、發明說明(8) 形成在某一端具有用以導入溶液之導入口 2〇7之導入 通路2 1 0以及在某一端具有用以排出溶液至系統外之排出 口 215之排出通路212 ·’使得該導入通路21〇和該排出通路 212交差於各個其他端而形成交差部214,同時,將具有在 该父差部2 1 4設置朝向基板2 0 1來成為開口狀之開口部2 〇 6 所構成之喷嘴構成體以及用以控制接觸到基板2〇1之溶液 壓力和大氣壓間之差異而透過該開口部2〇6來使得接觸到 基板201之溶液不流動至該排出通路212外之壓力控 213的喷嘴202,設置在前述溶解室6内 液導入口 9和該導入口 207,同砗、击# 乂 解用 排出口 215。壓力控制手段係可以介以 液排出口 1 0和該排出口 2 1 5間。 疋&解 在前述實施例,即使是在由溶 後,也會在溶解室6内’殘留溶解液。因此,導 =室來取出基板時之真空室之 二為由 空度之降低。 在:例子/合解用溶液係並無曝 ,中出因,,溶解液之回收係變得極為簡單。並且内之: ”解室來取出基板之狀態τ,也不會導 至之’::液所if之污染或真空度之降低。 洗淨基板表包富勒烯之溶解後,a會有必須 使得基板導入口板洗淨之洗淨室’200418723 V. Description of the invention (8) An introduction passage 2 1 0 having an introduction port 207 for introducing a solution at one end and an outlet passage 212 having an outlet 215 for discharging the solution to the outside of the system are formed at one end. 'The introduction passage 21o and the discharge passage 212 cross each other to form an intersection portion 214, and at the same time, an opening portion 2 is provided in the parent difference portion 2 1 4 to face the substrate 201 to form an opening. The nozzle structure formed by 6 and the difference between the pressure and the atmospheric pressure of the solution contacting the substrate 201 are controlled through the opening portion 206 so that the solution contacting the substrate 201 does not flow outside the discharge path 212 The nozzle 202 of the pressure control 213 is provided in the liquid introduction port 9 and the introduction port 207 in the dissolution chamber 6 in the same manner, and the discharge port 215 is pressed. The pressure control means may be between the liquid discharge port 10 and the discharge port 2 15. Solution & Solution In the foregoing embodiment, even after the dissolution, the dissolution solution remains in the dissolution chamber 6 '. Therefore, two of the vacuum chambers when the substrate is taken out of the chamber are caused by the decrease in vacancy. In: Example / Solution solution system is not exposed, the reason is out, the recovery system of the dissolved solution becomes extremely simple. And inside: "The state τ of the solution chamber to take out the substrate will not lead to the ':: contamination of the solution or the reduction of the vacuum degree. After the fullerene of the substrate is washed, the a will be necessary. Cleaning room for cleaning substrate introduction port plate '

2015-6047-PF(Nl).ptd 第13頁 200418723 五、發明說明(9) 然而’如果藉由溶液之切換而切換溶解用溶液和洗淨 液的話,則可以在溶解後,僅藉著使得導入液, 為純水或超純水,就已經足夠。也就是說’,即使 不设置洗淨室’也可以簡化用以能夠洗淨基板之 在圖2,符號202係濕式處理液供應嗔 喷嘴2。2係主要由喷嘴構成體25。和厂堅力控制里 在圖所示,壓力控制部213係藉由 =壓:浦所構成。也就是說,藉由控制減壓Λ之』 處理液…,進而控制大氣壓和接觸I,; 被u式處理物1間之濕式處理液之壓力間之差異。 隹减&幫浦217,控制吸引交差部214之渴 式,理液之力,得到溶液壓力(也包含㉟式處理液*面 濕式處理物之處理面之表面張力)和溶解室,面 t产理合广至矣内之軋讥之濕式處理液之壓力Pw (也包含渴 ί ί Ϊ 張力和被濕式處理物之處理面之表面張•力 206口 \解徂室内壓上間之關係’成為P,Pa而透過開口部、 206 ’來供應至基板201 ;接觸到基板2〇1之溶解用液係 ‘公' 至濕式處理液供應喷嘴之外部,排出至該排出通路 此外,如果作為交差部之頂部形狀係成為產生附壁效 200418723 五、發明說明(ίο) 果之形狀的話,則容易得到壓力之均衡,而變得更加理 想。 此外,在喷嘴之頂部218,設置超音波施加手段220。 可以藉由在溶解時,施加超音波而更加容易地由基板,來 脫離内包富勒烯。 當然,本發明係並非限定在以上敘述之實施例。 例如在圖1,使得保持體8成為上下地進行動作之縱型 樣式而說明裝置,但是,也可以使得圖1之裝置,成為傾 斜9 0度之橫型裝置。此外,也可以在承載器,能夠呈可變 地施加偏電壓。 【產業上之可利用性】 能夠以高生產效率,來製造高品質之内包富勒烯。2015-6047-PF (Nl) .ptd Page 13 200418723 V. Description of the invention (9) However, 'If the solution for dissolution and the washing solution are switched by switching the solution, after dissolving, only by making As the introduction liquid, pure water or ultrapure water is sufficient. That is, even if a cleaning chamber is not provided, it is possible to simplify the cleaning of the substrate. In Fig. 2, reference numeral 202 denotes a wet processing liquid supply 嗔 nozzle 2. The 2 is mainly composed of a nozzle body 25. As shown in the figure, the pressure control unit 213 is composed of = pressure: pu. That is, by controlling the pressure of the treatment liquid Λ, and then controlling the difference between the atmospheric pressure and the pressure of the wet treatment liquid between the treated objects 1; Reduce & pump 217, control the thirst type and fluid force of the suction cross section 214, and obtain the solution pressure (including the surface tension of the processing surface of the surface processing solution) and the dissolution chamber and surface. The pressure Pw of the wet processing fluid for rolling and processing in the production line (including 渴 ί ί tension and the surface tension of the treated surface of the wet-processed material) 206 ports \ The relationship 'becomes P, Pa, and is supplied to the substrate 201 through the openings, 206'; the dissolving liquid system 'male' contacting the substrate 201 is discharged to the outside of the wet processing liquid supply nozzle, and is discharged to the discharge path. If the shape of the top of the cross section is to produce the effect of Coanda 200418723 V. Description of Invention (ίο), it is easy to obtain the pressure balance and become more ideal. In addition, an ultrasonic wave is provided on the top 218 of the nozzle. Application means 220. The fullerene can be detached from the substrate more easily by applying an ultrasonic wave during dissolution. Of course, the present invention is not limited to the embodiment described above. For example, in FIG. 8 describes the device as a vertical type that moves up and down, but the device of FIG. 1 can also be made into a horizontal type with an angle of 90 degrees. In addition, a bias voltage can be applied to the carrier in a variable manner. [Industrial Applicability] It is possible to produce high-quality enclosed fullerenes with high production efficiency.

20!5-6047-PF(Nl).ptd 第15頁 200418723 圖式簡單說明 圖1係顯示實施例1之例子之剖面圖及俯視圖 圖2係顯示實施例2之例子之剖面圖。 【符號說明】20! 5-6047-PF (Nl) .ptd Page 15 200418723 Brief Description of Drawings Fig. 1 is a sectional view and a plan view showing an example of Embodiment 1 Fig. 2 is a sectional view of an example of Embodiment 2. 【Symbol Description】

Pa〜溶解室内壓; 1〜真空室; 2b〜基板導入口; 3 b〜基板; 4b〜承載器; 6〜溶解室; 9〜溶解用液導入口Pa ~ pressure in the dissolution chamber; 1 ~ vacuum chamber; 2b ~ substrate introduction port; 3b ~ substrate; 4b ~ carrier; 6 ~ dissolution chamber; 9 ~ dissolution liquid introduction port

Pw〜濕式處理液之壓力 2a〜基板導入口; 3 a〜基板; 4 a〜承載器; 5〜成膜室; 8〜保持體; ;1 0〜溶解用液排出口; 閥 閘 造 製 的 烯 勒 富 ., 包板 内基 二 11 ο ο 具 工 統 系 收 回 嘴 喷 應 供 液 JI 處 式 濕 2 ο 段 手 ; •’加 ;路;浦施 口通部幫波 入出差壓音 導排交減超一 一 一 一 一 7 2 4 7 0 11 1± 1i ox^_ 2 2 2 2 2 段 。 •,手 ·,體 ;路制;部成 部通控口頂構 口入力出嘴嘴 開導壓排喷喷二二二 6 0 3 5 8 0 Λυ 11 11 11 11Pw ~ pressure of wet processing liquid 2a ~ substrate introduction port; 3a ~ substrate; 4a ~ carrier; 5 ~ film forming chamber; 8 ~ holding body; 10 ~ dissolving liquid discharge port; valve gate manufacturing Erlefu., Cladding inner base II 11 ο ο The engineering system retracts the nozzle to spray the liquid supply JI virgin wet 2 ο segment hand; • 'plus; the road; the Pu Shi mouth through the Ministry of pressure in and out differential pressure sound Leading cross-over reduction one by one one by one 7 2 4 7 0 11 1 ± 1i ox ^ _ 2 2 2 2 2 paragraph. •, hand ·, body; road system; part-by-part, top-control mouth structure, mouth-in force, mouth-out, mouth opening, pressure-exhausting, spraying, spraying, spraying, spraying, spraying, spraying, spraying, spraying, spraying, spraying, spraying, spraying, spraying.

2015-6047-PF(Nl).ptd 第16頁2015-6047-PF (Nl) .ptd Page 16

Claims (1)

六、申請專利範圍 於包括:内包§勒烯的製造·回收李 真空室· 恭统工具,其特徵在 入 成膜室,在該真空室側,具有 溶解^進仃對於基板上之内包舍^導入基板之基板導 進行内Ξ;勒:該成膜室,於該真之堆積; 以導入來;勒細堆積之基板之基板導;:’具有用以導入 進仃堆積在基板上之内向含口,並且,具有用 =岭解用液導入口以及用以排:勒烯溶解用之溶解用 浴解用液(將該溶解用液稱為「、、4溶解内包富勒烯後之 口;以及。。 吟解液」)之溶解液排出 …承載器,能夠進行旋轉及往 複數個基板,能夠將基板導入至成=,並且,可以載置 ^ 2 ·如申請專利範圍第1項之内勺至或該溶解室。 系統工具,其中,前述内包富勒歸%萄八勒烯的製造•回收 3.如申請專利範圍第2項之内勺〃〜金屬内包富勒烯。 系統工具,其中,前述金屬係鹼金勒烯的製造•回收 4·如申請專利範圍第1至3項中二 製造·回收系統工具,《中,前述、:7項之内包富勒烯的 5 ·如申請專利範圍第1至4項中^ 用液係苯胺。 製造·回收系統工具,其中,形成壬:項之内包富勒烯的丨 入溶液之導入口之導入通路以及在羋端具有用以導 液至系統外之排出口之排出通路·佶—端具有用以排出溶 出通路交差於各個其他端而形成交】,該導入通路和該排 _ ,同時,將具有在 inn 2015-6047-PF(Nl).ptd $ 17頁6. The scope of applying for patents includes: manufacturing and recycling of olefins, vacuum vacuum chambers, and Gongtong tools, which are characterized in the film-forming chamber, and on the side of the vacuum chamber, there is a solution ^ into the inner package on the substrate ^ The substrate guide introduced into the substrate is internally inserted; Le: the film forming chamber is stacked in the true; the introduction is introduced; the substrate guide of the thinly stacked substrate is introduced; It also has an introduction port for lysing solution and a bathing solution for dissolving lerene (the dissolving solution is referred to as ",, 4 after dissolving the inclusion of fullerene); And ... Dissolving liquid discharge of the "infusion solution") ... The carrier can rotate and reciprocate several substrates, can introduce substrates into the =, and can be placed ^ 2 as within the scope of the first patent application Scoop into or the dissolution chamber. System tool, in which, the production and recycling of the aforementioned enclosed fullerene% octadecene 3. As in the scope of the patent application No. 2 ~ metal enclosed fullerene. System tools, in which the production and recycling of the aforementioned metal-based alkali metalloprene 4 · For example, in the scope of application for patents No. 1 to No. 3, manufacturing and recycling system tools, "Medium, the aforementioned ,: 7 of the fullerene 5 · As in the application of the scope of patent applications Nos. 1 to 4 ^ liquid aniline. Manufacturing and recycling system tools, in which the introduction path of the full solution-containing fullerene-introducing solution introduction port and the discharge path at the 芈 end for conducting liquid to the discharge port outside the system are provided. It is used to discharge the dissolution path to the other end to form an intersection], the introduction path and the row _, at the same time, will have inn 2015-6047-PF (Nl) .ptd $ 17 pages 200418723 六、申請專利範圍 該交差部設置朝向基板來成為開口狀之開口部所構成之喷 = 以控制接觸到基板之溶液壓力和大氣壓間 之差異而透過该開口部來使得接觸 :排=路夕之壓力控制手段的喷嘴,設置在 内,連接丽述溶解用液導入口和誃 =^述冷解至 述溶解液排出口和該排出口。 5日寸’連接如 “mr範圍第5項之内包富㈣的製造·回收 =中’設置用以賦予超音波至該溶解液之手 7·如申請專利範圍第5或6項之 收系統工具,其中,在前述溶解用液導二口之:ς造二回 切換閥,切換閥之某一邊係連接在 4,没置 接在洗淨液。 n—解W ’其他邊係連 8. 如申請專利範圍第1至7項中任— 製造·回收系統工具’其中,在前述成膜 ^勒烯的 間,設置用以洗淨溶解後之基板之洗^室。和别述溶解室 9. 如申請專利範圍第i至8項中任— 製造•回收系統工具,#中,在前述溶解 ;:$烯的 譜法用柱。 連接溶液色 10如申請專利範圍第9項之内包富勒 糸統工具,其中,在前述柱之下游,連 化·回收 1 1 ·如申請專利範圍第1 0項之内包含 刀析機态。 r統工具,其中’前述柱及成分分析=的配製造·回 真空室内。 乐配置在前述200418723 VI. Scope of patent application The intersection part is provided with an opening formed by openings facing toward the substrate to form an opening = to control the difference between the pressure of the solution in contact with the substrate and the atmospheric pressure, and to make contact through the opening: row = road evening The nozzle of the pressure control means is arranged inside, and connects the Lisu dissolving liquid introduction port and the 誃 = ^ lysis to the dissolving solution discharge port and the discharge port. 5-day inch 'connection such as "manufacturing and recycling of fufu in item 5 of the mr range = medium" is set to give ultrasound to the hand of the dissolving solution 7 · as in the patent application scope of item 5 or 6 of the collection system tool Among them, in the liquid dissolving two port of the aforementioned dissolving: make two switching valves, one side of the switching valve is connected to 4, and not connected to the washing liquid. N— 解 W 'Other sides are connected 8. Such as Any of the scope of applications for patents Nos. 1 to 7-manufacturing and recycling system tools' wherein, a washing chamber for cleaning the substrate after dissolution is provided between the aforementioned film-forming lerene. And other dissolution chamber 9. For example, any of the items i to 8 in the scope of the patent application — manufacturing and recycling system tools, #, in the aforementioned dissolution;: $ ene column for spectrometry. Connection solution color 10 as described in the scope of the patent application, including fuller 糸System tools, in which, downstream of the aforementioned column, Lianyungang · Recycling 1 1 · If the scope of the patent application scope includes the knife analysis machine state. R system tools, in which the aforementioned column and composition analysis = preparation manufacturing · Back to the vacuum chamber. 2015-6047-PF(Nl).ptd 第18頁2015-6047-PF (Nl) .ptd Page 18
TW092135886A 2002-12-16 2003-12-16 Involved fullerene manufacturing and collecting system tool TW200418723A (en)

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JP2002364410A JP3923007B2 (en) 2002-12-16 2002-12-16 Encapsulated fullerene production / recovery system tool

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JP5065681B2 (en) * 2004-08-04 2012-11-07 金子 博之 Induction fullerene production apparatus and production method, and induction fullerene
CN102126717B (en) * 2010-12-16 2012-11-21 中国科学院高能物理研究所 Fullerene oxygen-free collection mixer

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JPS59116372A (en) * 1982-12-23 1984-07-05 Hitachi Ltd Continuous vacuum treatment apparatus
JPH05116924A (en) * 1991-10-29 1993-05-14 Mitsui Eng & Shipbuild Co Ltd Device for producing fullerenes
JPH06183712A (en) * 1992-10-23 1994-07-05 Showa Denko Kk Production of fullerenes
JP2611179B2 (en) * 1994-02-25 1997-05-21 工業技術院長 Fullerene manufacturing method and apparatus
JP3418457B2 (en) * 1994-08-29 2003-06-23 財団法人宇宙環境利用推進センター Method for producing fullerenes
JPH09309711A (en) * 1996-03-18 1997-12-02 Toyo Tanso Kk Carbon cluster, raw material for producing the same and production of the same carbon cluster
JP2000159514A (en) * 1998-11-26 2000-06-13 Univ Nagoya Production of metal-including fullerene

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