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CN1951804A - Carbon nanotube preparation apparatus - Google Patents

Carbon nanotube preparation apparatus Download PDF

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CN1951804A
CN1951804A CNA2005101005874A CN200510100587A CN1951804A CN 1951804 A CN1951804 A CN 1951804A CN A2005101005874 A CNA2005101005874 A CN A2005101005874A CN 200510100587 A CN200510100587 A CN 200510100587A CN 1951804 A CN1951804 A CN 1951804A
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carbon nanotube
air inlet
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outlet
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CN100482584C (en
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萧博元
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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    • B82NANOTECHNOLOGY
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    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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Abstract

The invention discloses a preparing equipment of carbon nanometer pipe, which consists of reacting cavity and diversion device, wherein the reacting cavity contains the first inlet and outlet; the diversion device is set in the reacting cavity, which concludes gas transmitting pipe, second inlet and outlet; one end of gas transmitting pipe cases the first inlet closely and the other end cases the second inlet closely; the opening direction of second outlet is perpendicular to base of nanometer pipe; the second outlet lies on one side of second inlet; the second outlet connects the first outlet.

Description

碳纳米管制备设备Carbon nanotube preparation equipment

【技术领域】【Technical field】

本发明涉及一种碳纳米管的制备设备,尤其是一种热化学气相沉积的碳纳米管制备设备。The invention relates to a preparation device for carbon nanotubes, in particular to a preparation device for carbon nanotubes by thermal chemical vapor deposition.

【背景技术】【Background technique】

碳纳米管是一种新型一维奈米碳材料,由日本研究人员饭岛澄男(S.Iijima)于1991年首次发现。碳纳米管具有优异的性质,如高抗张强度与高热稳定性,并且随着碳纳米管螺旋方式的变化,碳纳米管可呈现出金属性或半导体性等。由于碳纳米管具有理想的一维结构以及在力学、电学、热学等领域优良的性质,其在材料科学、化学、物理学等交叉学科领域已展现出广阔的应用前景。因此,实现碳纳米管的可控生长,是将碳纳米管推向应用的关键。Carbon nanotubes are a new type of one-dimensional nanocarbon material, which was first discovered in 1991 by Japanese researcher Iijima Sumio (S.Iijima). Carbon nanotubes have excellent properties, such as high tensile strength and high thermal stability, and with the change of the helical mode of carbon nanotubes, carbon nanotubes can exhibit metallic or semiconducting properties. Because carbon nanotubes have an ideal one-dimensional structure and excellent properties in the fields of mechanics, electricity, and heat, they have shown broad application prospects in interdisciplinary fields such as materials science, chemistry, and physics. Therefore, realizing the controllable growth of carbon nanotubes is the key to promote the application of carbon nanotubes.

目前,较为常用的碳纳米管制备方法是化学气相沉积法。化学气相沉积法是利用含碳气体作为碳源气,在硅或沸石基底上生长出多壁或单壁碳纳米管。但是,如图1所示,现有技术中的热CVD碳纳米管制备设备1包括一石英管17,该石英管17包括一进气口13及一与该进气口13相对设置的出气口15。在碳纳米管的制备过程中,将一表面形成有催化剂层22的基底2装载在所述石英管17内,反应气体11由进气口13水平方向吹送至出气口15,即与碳纳米管的生长方向垂直。对于微细碳纳米管而言,即使该反应气体的流速缓慢,其也将使得最终生长出的碳纳米管准直性不佳。At present, the more commonly used method for preparing carbon nanotubes is chemical vapor deposition. The chemical vapor deposition method uses carbon-containing gas as a carbon source gas to grow multi-walled or single-walled carbon nanotubes on silicon or zeolite substrates. But, as shown in Figure 1, thermal CVD carbon nanotube preparation equipment 1 in the prior art comprises a quartz tube 17, and this quartz tube 17 comprises an air inlet 13 and a gas outlet that is arranged opposite to this air inlet 13 15. In the preparation process of carbon nanotubes, a substrate 2 with a catalyst layer 22 formed on the surface is loaded in the quartz tube 17, and the reaction gas 11 is blown from the gas inlet 13 to the gas outlet 15 in the horizontal direction, that is, it is mixed with the carbon nanotubes. The growth direction is vertical. For fine carbon nanotubes, even if the flow rate of the reaction gas is slow, it will lead to poor alignment of the finally grown carbon nanotubes.

有鉴于此,提供一种可生长准直性碳纳米管的制备设备实为必要。In view of this, it is necessary to provide a preparation device capable of growing aligned carbon nanotubes.

【发明内容】【Content of invention】

下面将以实施例说明一种碳纳米管的制备设备,其可实现碳纳米管的准直性生长。A carbon nanotube preparation device will be described below with examples, which can realize the collimated growth of carbon nanotubes.

一种碳纳米管的制备设备,其包括一反应腔及一导流装置。该反应腔包括一第一进气口及一第一出气口。该导流装置位于该反应腔内,其包括一气体输送管、一第二进气口及一第二出气口,其中该气体输送管一端与所述第一进气口密封套接,另一端与所述第二进气口密封套接,该第二进气口的开口方向垂直于用于生长碳纳米管的基底设置,该第二出气口位于该第二进气口相对的一侧,该第二出气口与该第一出气口导通。A preparation device for carbon nanotubes, which includes a reaction chamber and a flow guiding device. The reaction chamber includes a first gas inlet and a first gas outlet. The flow guiding device is located in the reaction chamber, and it includes a gas delivery tube, a second gas inlet and a second gas outlet, wherein one end of the gas delivery tube is sealed and sleeved with the first gas inlet, and the other end is Sealed with the second air inlet, the opening direction of the second air inlet is set perpendicular to the substrate for growing carbon nanotubes, the second air outlet is located on the opposite side of the second air inlet, The second air outlet communicates with the first air outlet.

与现有技术相比较,所述碳纳米管制备设备,其通过采用导流装置改变碳纳米管生长所需的反应气体流向,使该流向由现有技术中的垂直碳纳米管生长方向转为平行于碳纳米管生长方向,该种设置可以使碳纳米管具有较佳的准直性。Compared with the prior art, the carbon nanotube preparation equipment uses a diversion device to change the flow direction of the reaction gas required for the growth of the carbon nanotubes, so that the flow direction is changed from the vertical carbon nanotube growth direction in the prior art to Parallel to the growth direction of the carbon nanotubes, this arrangement can make the carbon nanotubes have better alignment.

【附图说明】【Description of drawings】

图1是现有技术中的碳纳米管制备设备的结构示意图。Fig. 1 is a schematic structural diagram of a carbon nanotube preparation equipment in the prior art.

图2是本发明第一实施例的碳纳米管制备设备的结构示意图。Fig. 2 is a schematic structural diagram of a carbon nanotube preparation device according to the first embodiment of the present invention.

图3是本发明第二实施例的碳纳米管制备设备的结构示意图。Fig. 3 is a schematic structural diagram of a carbon nanotube preparation device according to a second embodiment of the present invention.

【具体实施方式】【Detailed ways】

下面结合附图将对本发明实施例作进一步详细的说明。The embodiments of the present invention will be further described in detail below in conjunction with the accompanying drawings.

参见图2,本发明第一实施例所提供的碳纳米管制备设备10,其包括一反应腔20、一导流装置30以及一加热装置12,其中该导流装置30设置于该反应腔20内。Referring to FIG. 2, the carbon nanotube preparation equipment 10 provided by the first embodiment of the present invention includes a reaction chamber 20, a flow guide device 30 and a heating device 12, wherein the flow guide device 30 is arranged in the reaction chamber 20 Inside.

该反应腔20包括第一进气口22及第一出气口24,该反应腔20可选用石英管。The reaction chamber 20 includes a first gas inlet 22 and a first gas outlet 24, and the reaction chamber 20 can be a quartz tube.

该导流装置30包括一气体输送管32、一第二进气口34以及一第二出气口36。本实施例中,该导流装置30除气体输送管32外的部分呈无底面的槽体结构,其材质可选用导热材料,如不锈钢。该气体输送管32一端与所述第一进气口22密封套接,另一端与第二进气口34密封套接。该气体输送管32可包括一弯折段,通过该弯折段可使第一进气口22与第二进气口34的开口方向处于垂直状态。该第二进气口34的开口方向相对于生长碳纳米管的基底40垂直设置,本实施例中该第二进气口34设置在基底40的上方部位并与基底垂直。该第二出气口36位于该第二进气口34相对一侧的导流装置30的底部,该第二出气口36的开口方向与所述第一进气口22的开口方向平行。也可以将第二出气口36设置在该第二进气口34相对一侧的导流装置30的底部,且使其开口方向与所述第一进气口22的开口方向垂直的位置,只要使该第二出气口36邻近基底40的位置均可。The flow guiding device 30 includes a gas delivery tube 32 , a second gas inlet 34 and a second gas outlet 36 . In this embodiment, the part of the flow guiding device 30 except the gas delivery pipe 32 is a tank structure without a bottom surface, and its material can be made of heat-conducting materials, such as stainless steel. One end of the gas delivery pipe 32 is tightly socketed with the first air inlet 22 , and the other end is airtightly socketed with the second air inlet 34 . The gas delivery pipe 32 may include a bent section, through which the opening directions of the first air inlet 22 and the second air inlet 34 can be in a vertical state. The opening direction of the second gas inlet 34 is set vertically relative to the substrate 40 for growing carbon nanotubes. In this embodiment, the second gas inlet 34 is arranged above the substrate 40 and perpendicular to the substrate. The second air outlet 36 is located at the bottom of the deflector 30 opposite to the second air inlet 34 , and the opening direction of the second air outlet 36 is parallel to the opening direction of the first air inlet 22 . It is also possible to arrange the second air outlet 36 at the bottom of the deflector 30 on the opposite side of the second air inlet 34, and make its opening direction perpendicular to the opening direction of the first air inlet 22, as long as Any position where the second air outlet 36 is adjacent to the base 40 is acceptable.

该加热装置12设置于反应腔20之周围,用于对装载于反应腔20内之奈米碳管生长用催化剂层50进行加热。该加热装置12可选用高温炉及高频炉等加热设备。The heating device 12 is disposed around the reaction chamber 20 for heating the catalyst layer 50 for growing carbon nanotubes loaded in the reaction chamber 20 . The heating device 12 can be selected from heating equipment such as a high-temperature furnace and a high-frequency furnace.

下面结合碳纳米管的制备过程详细说明本实施例所提供的碳纳米管制备设备10的使用方法。The method of using the carbon nanotube preparation device 10 provided in this embodiment will be described in detail below in conjunction with the preparation process of carbon nanotubes.

参见图2,先将一基底40放入反应腔20内,该基底40表面形成有一催化剂层50,设置好导流装置20使其完全包围该基底40。该基底40可选用石英、硅、氧化镁等基片。该催化剂层50可选用钴、镍、铁,或其合金材料。由于该导流装置30采用无底面的槽体结构,从而将第二出气口36设置在导流装置20底部且其开口方向与第一进气口22的开口方向平行的位置。Referring to FIG. 2 , a substrate 40 is first put into the reaction chamber 20 , a catalyst layer 50 is formed on the surface of the substrate 40 , and the flow guiding device 20 is arranged to completely surround the substrate 40 . The substrate 40 can be selected from quartz, silicon, magnesium oxide and other substrates. The catalyst layer 50 can be made of cobalt, nickel, iron, or alloy materials thereof. Since the flow guiding device 30 adopts a bottomless groove structure, the second air outlet 36 is arranged at the bottom of the flow guiding device 20 and its opening direction is parallel to the opening direction of the first air inlet 22 .

然后,在常压下从第一进气口22通入载气气体,该载气气体通过气体输送管32及第二进气口34,从导流装置30的顶部进入其内并垂直吹向基底40。该载气气体可选用氢气、氮气、氨气或其它惰性气体等。通过加热装置12对反应腔20内的催化剂层50进行加热。待催化剂层50的温度升高至预定温度后,一般为500度~900度,从第一进气口22通入反应气体。所述反应气体可选用甲烷、乙烷、乙烯、乙炔等碳源气。该反应气体经气体输送管32及第二进气口34进入导流装置30内。由于催化剂的催化作用,通入到反应腔20的碳源气热分解成碳单元与氢气,碳单元吸附到催化剂层50形成的催化剂颗粒表面,待催化剂颗粒中吸附的碳单元达到饱和后将析出,从而可在催化剂颗粒位置生长出碳纳米管。而载气气体与反应后产生的废气可通过第二出气口36及与其导通的第一出气口24排出。该第二出气口36与第一出气口24可通过一导管连接,使载气气体与反应后产生的废气直接从第二出气口36到第一出气口24并排出,也可以不使用导管连接,将载气气体与反应后产生的废气直接从第二出气口36排出到反应腔20内,再通过气体的流动从第一出气口24排出。Then, under normal pressure, the carrier gas is passed from the first air inlet 22, the carrier gas passes through the gas delivery pipe 32 and the second air inlet 34, enters it from the top of the flow guiding device 30 and blows it vertically Base 40. The carrier gas may be hydrogen, nitrogen, ammonia or other inert gases. The catalyst layer 50 in the reaction chamber 20 is heated by the heating device 12 . After the temperature of the catalyst layer 50 rises to a predetermined temperature, generally 500°C to 900°C, the reaction gas is introduced from the first air inlet 22 . The reaction gas can be selected from carbon source gases such as methane, ethane, ethylene, acetylene and the like. The reaction gas enters the flow guide device 30 through the gas delivery pipe 32 and the second gas inlet 34 . Due to the catalytic effect of the catalyst, the carbon source gas passed into the reaction chamber 20 is thermally decomposed into carbon units and hydrogen gas, and the carbon units are adsorbed on the surface of the catalyst particles formed by the catalyst layer 50, and will be precipitated after the carbon units adsorbed in the catalyst particles reach saturation. , so that carbon nanotubes can be grown at the position of catalyst particles. The waste gas generated after the reaction between the carrier gas and the reaction can be discharged through the second gas outlet 36 and the first gas outlet 24 connected thereto. The second gas outlet 36 and the first gas outlet 24 can be connected through a conduit, so that the carrier gas and the waste gas generated after the reaction are directly discharged from the second gas outlet 36 to the first gas outlet 24, or no conduit can be used. , the carrier gas and the waste gas generated after the reaction are directly discharged into the reaction chamber 20 from the second gas outlet 36 , and then discharged from the first gas outlet 24 through the flow of the gas.

如图3所示,本发明第二实施例中碳纳米管制备设备100包括一加热装置120、一反应腔200及一导流装置300,其中该导流装置300可选用具有底面的箱体结构。此时,该导流装置300的气体输送管320的一端与第一进气口220密封套接,另一端与第二进气口340密封套接;该导流装置300的第二进气口340位于导流装置300的顶部,第二出气口360可设置在该导流装置300的底部且其开口方向与第一进气口220的开口方向垂直的位置,还可以将第二出气口360设置在该导流装置300的底部且其开口方向与第一进气口220的开口方向平行的位置,即相对于该第二进气口340的位置,只要使该第二出气口360邻近基底400的位置均可。As shown in Figure 3, the carbon nanotube production equipment 100 in the second embodiment of the present invention includes a heating device 120, a reaction chamber 200 and a flow guide device 300, wherein the flow guide device 300 can be selected as a box structure with a bottom surface . At this time, one end of the gas delivery pipe 320 of the flow guiding device 300 is tightly socketed with the first air inlet 220, and the other end is tightly socketed with the second air inlet 340; the second air inlet of the flow guiding device 300 340 is located at the top of the air guiding device 300, the second air outlet 360 can be arranged at the bottom of the air guiding device 300 and its opening direction is perpendicular to the opening direction of the first air inlet 220, and the second air outlet 360 can also be It is arranged at the bottom of the flow guiding device 300 and its opening direction is parallel to the opening direction of the first air inlet 220, that is, relative to the position of the second air inlet 340, as long as the second air outlet 360 is adjacent to the base 400 positions are available.

本发明第二实施例中,可将形成有催化剂层500的基底400直接放入导流装置300内,并将其导流装置300放入反应腔200内即可。也可附加一承载装置600,用于支撑基底400,并调整该基底400与第二进气口340之间的距离。而制备碳纳米管的其它步骤则与第一实施例相同。In the second embodiment of the present invention, the substrate 400 formed with the catalyst layer 500 can be directly put into the flow guiding device 300 , and the flow guiding device 300 can be put into the reaction chamber 200 . A carrying device 600 can also be added to support the base 400 and adjust the distance between the base 400 and the second air inlet 340 . Other steps of preparing carbon nanotubes are the same as those in the first embodiment.

可以理解的是,在本发明实施例中如所述第一进气口与第二进气口的开口方向之间、第一进气口与第二出气口的开口方向之间、及第一进气口的开口方向与基底之间的位置关系并不限于绝对的平行或垂直,只要能实现本发明的目的即可。It can be understood that, in the embodiment of the present invention, such as between the opening direction of the first air inlet and the second air inlet, between the opening direction of the first air inlet and the second air outlet, and the first The positional relationship between the opening direction of the air inlet and the base is not limited to being absolutely parallel or perpendicular, as long as the purpose of the present invention can be achieved.

本发明实施例所提供的碳纳米管制备设备,其通过导流装置改变碳纳米管生长用反应气体的流向,使其与碳纳米管得生长方向平行,进而可实现准直性碳纳米管的制备。The carbon nanotube preparation equipment provided by the embodiment of the present invention changes the flow direction of the reaction gas used for carbon nanotube growth through a flow guiding device so that it is parallel to the growth direction of carbon nanotubes, thereby realizing the alignment of carbon nanotubes preparation.

另外,本领域技术人员还可在本发明精神内做其它变化,如适当变化导流装置的形状及设置位置,或改变导流装置的进气口及出气口的设置位置,只要其不偏离本发明的实施效果即可。这些依据本发明精神所做的变化,都应包含在本发明所要求保护的范围的内。In addition, those skilled in the art can also make other changes within the spirit of the present invention, such as appropriately changing the shape and setting position of the flow guiding device, or changing the setting positions of the air inlet and the air outlet of the flow guiding device, as long as it does not deviate from the present invention. The implementation effect of the invention is enough. These changes made according to the spirit of the present invention should be included in the scope of the present invention.

Claims (8)

1.一种碳纳米管制备设备,其包括一反应腔,该反应腔包括一第一进气口及一第一出气口,其特征在于进一步包括:1. A kind of carbon nanotube preparation equipment, it comprises a reaction chamber, and this reaction chamber comprises a first air inlet and a first gas outlet, it is characterized in that further comprising: 一导流装置,其设置在该反应腔内,a flow guiding device, which is arranged in the reaction chamber, 该导流装置包括一气体输送管,一第二进气口及以一第二出气口,该气体输送管一端与第一进气口密封套接,另一端与第二进气口密封套接,该第二进气口的开口方向垂直于用于生长碳纳米管的基底设置,该第二出气口位于该第二进气口相对的一侧,该第二出气口与该第一出气口导通。The flow guiding device includes a gas conveying pipe, a second air inlet and a second air outlet, one end of the gas conveying pipe is sealed and sleeved with the first air inlet, and the other end is sealed and sleeved with the second air inlet , the opening direction of the second air inlet is perpendicular to the substrate for growing carbon nanotubes, the second air outlet is located on the opposite side of the second air inlet, and the second air outlet is connected to the first air outlet conduction. 2.如权利要求1所述的碳纳米管制备设备,其特征在于所述反应腔为一石英管。2. The carbon nanotube preparation equipment according to claim 1, characterized in that the reaction chamber is a quartz tube. 3.如权利要求1所述的碳纳米管制备设备,其特征在于所述气体输送管包括一弯折段,使所述第一进气口与第二进气口的开口方向垂直。3 . The carbon nanotube preparation equipment according to claim 1 , wherein the gas delivery pipe comprises a bent section, so that the opening direction of the first gas inlet is perpendicular to the opening direction of the second gas inlet. 4 . 4.如权利要求1所述的碳纳米管制备设备,其特征在于所述第二出气口的开口方向与所述第一进气口的开口方向平行。4. The carbon nanotube production equipment according to claim 1, characterized in that the opening direction of the second gas outlet is parallel to the opening direction of the first gas inlet. 5.如权利要求1所述的碳纳米管制备设备,其特征在于所述第二出气口的开口方向与所述第一进气口的开口方向垂直。5 . The carbon nanotube preparation device according to claim 1 , wherein the opening direction of the second gas outlet is perpendicular to the opening direction of the first air inlet. 6.如权利要求1所述的碳纳米管制备设备,其特征在于所述导流装置是由导热材料所形成。6 . The carbon nanotube production equipment as claimed in claim 1 , wherein the flow guiding device is formed of a heat conducting material. 7 . 7.如权利要求6所述的碳纳米管制备设备,其特征在于所述导热材料包括不锈钢。7. The carbon nanotube production equipment as claimed in claim 6, characterized in that said thermally conductive material comprises stainless steel. 8.如权利要求1所述的碳纳米管制备设备,该设备进一步包括一承载装置,用于支撑所述基底,以调整第二进气口与基底之间的距离。8. The carbon nanotube preparation apparatus according to claim 1, further comprising a supporting device for supporting the substrate so as to adjust the distance between the second gas inlet and the substrate.
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