JPH0681218A - Graphitized vapor-grown carbon fiber for forming interlaminar compound and its production - Google Patents
Graphitized vapor-grown carbon fiber for forming interlaminar compound and its productionInfo
- Publication number
- JPH0681218A JPH0681218A JP23318492A JP23318492A JPH0681218A JP H0681218 A JPH0681218 A JP H0681218A JP 23318492 A JP23318492 A JP 23318492A JP 23318492 A JP23318492 A JP 23318492A JP H0681218 A JPH0681218 A JP H0681218A
- Authority
- JP
- Japan
- Prior art keywords
- carbon fiber
- grown carbon
- vapor
- graphitized
- intercalation compound
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は層間化合物形成用黒鉛
化気相成長炭素繊維及びその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a graphitized vapor grown carbon fiber for forming an intercalation compound and a method for producing the same.
【０００２】[0002]
【従来の技術と発明が解決しようとする課題】気相成長
炭素繊維は、超微粒子状の鉄やニッケルなどの金属を触
媒として炭素化合物を８００〜１，３００℃に加熱する
ことにより、これを熱分解して製造することができる。
この気相成長炭素繊維は熱処理することにより容易に黒
鉛構造に転化する特長を有している。例えば、この気相
成長炭素繊維を２，８００℃以上で加熱処理して得られ
た黒鉛化気相成長炭素繊維は、結晶欠陥の少ない黒鉛網
面が繊維軸に平行に発達している。したがって、この黒
鉛化気相成長炭素繊維は、層間化合物のホスト用材料と
して好適な材料であるとして期待されている。2. Description of the Related Art Vapor-grown carbon fibers are prepared by heating a carbon compound to 800 to 1300 ° C. using a metal such as iron or nickel in the form of ultrafine particles as a catalyst. It can be produced by thermal decomposition.
This vapor grown carbon fiber has a feature that it is easily converted into a graphite structure by heat treatment. For example, in the graphitized vapor-grown carbon fiber obtained by heating the vapor-grown carbon fiber at 2,800 ° C. or higher, the graphite network surface with few crystal defects develops parallel to the fiber axis. Therefore, this graphitized vapor grown carbon fiber is expected to be a material suitable as a host material for an intercalation compound.
【０００３】しかしながら、この発明者らの検討の結
果、黒鉛化気相成長炭素繊維をホスト材料として層間化
合物を製造したとき、層間化合物の生成速度が遅いとい
った問題が明らかになった。その理由は、以下のようで
あると、この発明者らは推定している。However, as a result of the investigations by the present inventors, when the intercalation compound was produced by using the graphitized vapor-grown carbon fiber as the host material, it became clear that the formation rate of the intercalation compound was slow. The present inventors presume that the reason is as follows.
【０００４】流動気相法により生成した気相成長炭素繊
維は、繊維の両端が丸く炭素の層で覆われているため
に、層間化合物のホスト材料として使用する場合、繊維
を粉砕し、切断する必要があった。Since vapor grown carbon fibers produced by the fluidized vapor phase method are rounded at both ends of the fibers and covered with a layer of carbon, the fibers are crushed and cut when used as a host material for an intercalation compound. There was a need.
【０００５】また、黒鉛化処理は気相成長炭素繊維を通
気性のある耐熱容器に詰めて、不活性気体を流した２，
０００℃以上の黒鉛化炉を通過させるのであるが、製造
されたままの気相成長炭素繊維は嵩高くて容器に充填で
きる量が少ないので、ハイブリダイザーやボールミルな
どによって、所定の長さに粉砕してから黒鉛化するのが
普通であった。Further, in the graphitization treatment, vapor-grown carbon fibers were packed in a gas proof heat-resistant container and an inert gas was flowed.
Although it is passed through a graphitization furnace at 000 ° C or higher, the vapor-grown carbon fiber as produced is bulky and the amount that can be filled in the container is small, so pulverize it to a predetermined length with a hybridizer or ball mill. It was normal to graphitize after that.
【０００６】このように気相成長炭素繊維を粉砕した後
に、黒鉛化した場合、その端面の炭素原子は再結合す
る。このとき、これらの炭素原子のいくつかが層間化合
物のゲスト材料の層間への進入を防げるように結合して
いると考えられる。When the vapor grown carbon fiber is crushed and then graphitized, the carbon atoms on the end face are recombined. At this time, it is considered that some of these carbon atoms are bonded so as to prevent the intercalation compound from entering the interlayer of the guest material.
【０００７】また、その雰囲気中に存在するフリーカー
ボンがその端面を覆うように結合していることなども考
えられる。It is also conceivable that the free carbon existing in the atmosphere is bonded so as to cover the end face.
【０００８】この発明は実質的に粉砕しない気相成長炭
素繊維を黒鉛化し、その後に所定の長さに粉砕した黒鉛
化気相成長炭素繊維を用い、層間化合物を製造したとこ
ろ、その反応速度が格段に改善され、粉砕、切断後に黒
鉛化処理した黒鉛化気相成長炭素繊維より勝れているこ
とを見いだしてこの発明に達した。すなわち、この発明
は黒鉛層間化合物のホスト材料に好適な黒鉛化気相成長
炭素繊維及びその製造方法を提供することにある。According to the present invention, an intercalation compound is produced using graphitized vapor-grown carbon fiber which has been substantially pulverized and then graphitized to a predetermined length. The present invention has been achieved by finding that it is significantly improved and is superior to the graphitized vapor grown carbon fiber that is graphitized after crushing and cutting. That is, the present invention provides a graphitized vapor-grown carbon fiber suitable as a host material for a graphite intercalation compound and a method for producing the same.
【０００９】[0009]
【前記課題を解決するための手段】前記課題を解決する
ための本願請求項１に記載の発明は、気相成長炭素繊維
を実質的に黒鉛化処理した後に粉砕してなることを特徴
とする層間化合物形成用黒鉛化気相成長炭素繊維であ
り、請求項２に記載の発明は、直径が５μｍ以下、アス
ペクト比が５０以下である前記請求項１に記載の層間化
合物形成用黒鉛化気相成長炭素繊維であり、請求項３に
記載の発明は、気相成長炭素繊維を実質的に黒鉛化処理
した後に粉砕することを特徴とする層間化合物形成用黒
鉛化気相成長炭素繊維である。The invention according to claim 1 for solving the above-mentioned problems is characterized in that vapor-grown carbon fibers are substantially graphitized and then pulverized. A graphitized vapor grown carbon fiber for forming an intercalation compound, wherein the invention according to claim 2 has a diameter of 5 μm or less and an aspect ratio of 50 or less. It is a grown carbon fiber, and the invention according to claim 3 is a graphitized vapor grown carbon fiber for forming an intercalation compound, characterized in that the vapor grown carbon fiber is substantially graphitized and then pulverized.
【００１０】−層間化合物形成用気相成長炭素繊維及び
その製造方法− この発明の層間化合物形成用気相成長炭素は、気相成長
炭素繊維を実質的に黒鉛化処理した後に粉砕されてな
る。-Vapor grown carbon fiber for forming intercalation compound and method for producing the same-The vapor grown carbon for forming intercalation compound of the present invention is obtained by substantially graphitizing the vapor grown carbon fiber and then pulverizing the carbon fiber.
【００１１】ここで、気相成長炭素繊維は、気相成長法
により製造することができる。Here, the vapor grown carbon fiber can be produced by a vapor growth method.
【００１２】気相成長法により気相成長炭素繊維を製造
する方法としては、いわゆる基板法と流動気相法とがあ
る。基板法は、基板に触媒金属例えば遷移金属もしくは
遷移金属化合物を担持させ、高温度に加熱しながら、そ
の基板上に炭素源ガスである炭化水素ガスを流通させる
ことにより、基板表面に炭素繊維を生成させる方法であ
り、流動気相法は、基板を使用せず、触媒金属になり得
る金属化合物を炭素源である炭素化合物とを気化して高
温の反応管中に流通させることにより、空間中に炭素繊
維を生成させる方法である。As a method for producing a vapor grown carbon fiber by the vapor growth method, there are a so-called substrate method and a fluidized vapor phase method. In the substrate method, a catalyst metal such as a transition metal or a transition metal compound is supported on the substrate, and while heating to a high temperature, a hydrocarbon gas that is a carbon source gas is circulated on the substrate to form carbon fibers on the substrate surface. The fluidized gas phase method is a method of producing a metal compound that can be a catalyst metal without using a substrate, by vaporizing a metal compound that is a carbon source into a reaction tube at a high temperature, This is a method of producing carbon fiber.
【００１３】具体的には、特開昭５２−１０７３２０
号、特開昭５７−１１７６２２号、特開昭５８−１５６
５１２号、特開昭５８−１８０６１５号、特開昭６０−
１８５８１８号、特開昭６０−２２４８１５号、特開昭
６０−２３１８２１号、特開昭６１−１３２６３０号、
特開昭６１−１３２６００号、特開昭６１−１３２６６
３号、特開昭６１−２２５３１９号、特開昭６１−２２
５３２２号、特開昭６１−２２５３２５号、特開昭６１
−２２５３２７号、特開昭６１−２２５３２８号、特開
昭６１−２２７５４２５号、特開昭６１−２８２４２７
号の各公報に記載の方法により製造される気相成長炭素
繊維をこの発明の方法における原料として使用すること
ができる。Specifically, Japanese Patent Laid-Open No. 52-107320
No. 57-176622 and 58-156.
512, JP-A-58-180615, JP-A-60-
185818, JP-A-60-224815, JP-A-60-231821, JP-A-61-132630,
JP-A-61-132600, JP-A-61-132666
3, JP-A-61-225319, JP-A-61-222.
5322, JP-A-61-225325, JP-A-61
-225327, JP-A-61-225328, JP-A-61-2275425, and JP-A-61-282427.
The vapor-grown carbon fibers produced by the method described in each of the publications can be used as a raw material in the method of the present invention.
【００１４】気相成長炭素繊維は実質的に粉砕、切断さ
れることなく黒鉛化処理がなされる。ここで、実質的に
粉砕、切断されることがないとは、切断面の形成が黒鉛
化後に行われると言う意味であって、黒鉛化処理に供さ
れる気相成長炭素繊維の粉砕、切断を全く行わないこと
ではない。つまり、場合によっては、気相成長炭素繊維
の予備的な粉砕、切断を行っても良い。ただし、この予
備的な粉砕、切断はできるだけ軽くしておくのが好まし
い。The vapor grown carbon fiber is graphitized without being substantially crushed and cut. Here, substantially not crushed and cut means that the formation of the cut surface is performed after graphitization, and the crushing and cutting of the vapor-grown carbon fiber to be subjected to the graphitization treatment. Is not to do at all. That is, in some cases, preliminary pulverization and cutting of the vapor grown carbon fiber may be performed. However, it is preferable to make this preliminary crushing and cutting as light as possible.
【００１５】黒鉛化処理は、気相成長炭素繊維を２，０
００℃以上、好ましくは２，５００℃以上、さらに好ま
しくは２，８００℃以上に加熱処理することを内容と
し、これによって黒鉛化気相成長炭素繊維を得ることが
できる。The graphitization treatment was carried out by using a vapor-grown carbon fiber of 2,0
The heat treatment is performed at a temperature of 00 ° C. or higher, preferably 2,500 ° C. or higher, more preferably 2,800 ° C. or higher, whereby a graphitized vapor grown carbon fiber can be obtained.
【００１６】得られる黒鉛化気相成長炭素繊維のｄ002
が３．４５〜３．３５Å、好ましくは３．４２〜３．３
５、更に好ましくは３．３７〜３．３５Åになるよう
に、Ｌｃが３０Å以上、好ましくは３００Å以上、更に
好ましくは１，０００Å以上になるように黒鉛化処理の
条件を適宜に設定するのが良い。ｄ002 が大きすぎた
り、Ｌｃが小さすぎたりする場合は、この黒鉛化気相成
長炭素繊維を用いても層間化合物を好適に得ることがで
きないことがある。D 002 of the resulting graphitized vapor grown carbon fiber
Is 3.45 to 3.35Å, preferably 3.42 to 3.3.
5, more preferably, the Lc is 30 Å or more, preferably 300 Å or more, and more preferably 1,000 Å or more so that Lc is 3.37 to 3.35 Å. good. If d 002 is too large or Lc is too small, it may not be possible to obtain an intercalation compound suitably even if this graphitized vapor grown carbon fiber is used.
【００１７】得られた黒鉛化気相成長炭素繊維は、次に
アスペクト比を下げるために粉砕される。粉砕手段に限
定はないが、小球体と供に撹乱するアクアマイザー（登
録商標）やボールミル、ジェットミルでもよいが、気流
中で激しく撹拌して、繊維と撹拌羽や壁と、また、繊維
同志を衝突させて粉砕するハイブリダイザーに黒鉛化気
相成長炭素繊維単独を装填し、処理するのがが好まし
い。黒鉛化気相成長炭素繊維のハイブリダイザー中にお
ける滞在時間、撹拌羽の回転数により繊維長さを調整す
ることができる。なお、粉砕時に繊維温度が２００℃以
上に上がるのは好ましくない。そこで、粉砕手段には適
宜の冷却手段を設けておくのが好ましい。The graphitized vapor grown carbon fiber obtained is then ground to reduce the aspect ratio. The crushing means is not limited, and may be an aquamizer (registered trademark), a ball mill, or a jet mill that is disturbed together with small spheres. It is preferable to load the hybridizer, which is crushed by colliding with, with the graphitized vapor-grown carbon fiber alone and then treated. The length of the graphitized vapor-grown carbon fiber in the hybridizer can be adjusted by adjusting the length of stay of the carbon fiber in the hybridizer and the rotation speed of the stirring blade. In addition, it is not preferable that the fiber temperature rises to 200 ° C. or more during pulverization. Therefore, it is preferable to provide an appropriate cooling means in the crushing means.
【００１８】この発明の黒鉛化気相成長炭素繊維は、前
記した粉砕手段によって所定の長さに調整されてなる。
この場合、所定の長さとして直径が５μｍ以下、好まし
くは０．１〜３μｍ以下であり、アスペクト比が５０以
下、好ましくは２０以下であるのが望ましい。直径が５
μｍを越えると、層間化合物形成用黒鉛化気相成長炭素
繊維を用いて層間化合物を形成したときに、繊維に割れ
が生じ易くなり、直径が０．１μｍ未満であると、層間
化合物の形成速度が遅くなる。また、平均アスペクト比
が５０以上であると層間化合物のゲスト材料の層間での
移動距離が長くなり、層間化合物の形成速度が遅くな
る。The graphitized vapor grown carbon fiber of the present invention is adjusted to a predetermined length by the above-mentioned pulverizing means.
In this case, it is desirable that the predetermined length has a diameter of 5 μm or less, preferably 0.1 to 3 μm or less, and an aspect ratio of 50 or less, preferably 20 or less. Diameter is 5
If the diameter exceeds 0.1 μm, when the intercalation compound is formed using the graphitized vapor grown carbon fiber for forming an intercalation compound, the fiber is likely to crack, and if the diameter is less than 0.1 μm, the formation rate of the intercalation compound is increased. Will be late. Further, if the average aspect ratio is 50 or more, the movement distance of the guest material of the intercalation compound between the layers becomes long, and the formation rate of the intercalation compound becomes slow.
【００１９】又、この粉砕処理によって生じた、黒鉛化
気相成長炭素繊維における新しい端面の割合が、全端面
の５０％以上であり、好ましくは６５％以上であるのが
良い。The proportion of new end faces in the graphitized vapor-grown carbon fiber produced by this pulverization treatment is preferably 50% or more, and more preferably 65% or more of the total end faces.
【００２０】−層間化合物− 本発明に用いる上記ゲスト材料としては、たとえばＬ
ｉ、Ｋ、Ｃｓ等のアルカリ金属、Ｃａ等のアルカリ土類
金属、Ｂｒ2 、Ｃｌ2 等のハロゲン、Ｈ2 ＳＯ4、ＨＮ
Ｏ3 等の無機酸、ＦｅＣｌ3 、ＦｅＢｒ3 、ＮｉＣｌ
2 、ＣｕＣｌ2 等のハロゲン化金属などがある。これら
の中でも、取り扱い易さの点では、ハロゲン化金属が好
ましい。なお、ゲスト材料が非ガス体であるときは、ゲ
スト材料とホスト材料としての層間化合物形成用気相成
長炭素繊維とは反応炉内で別々に存在させるのがよい。-Intercalation Compound- The guest material used in the present invention is, for example, L.
Alkali metals such as i, K and Cs, alkaline earth metals such as Ca, halogens such as Br 2 and Cl 2 , H 2 SO 4 and HN
Inorganic acids such as O 3 , FeCl 3 , FeBr 3 , NiCl
2 , and metal halides such as CuCl 2 . Among these, metal halides are preferable from the viewpoint of easy handling. When the guest material is a non-gaseous material, it is preferable that the guest material and the vapor-grown carbon fiber for forming an intercalation compound as the host material are separately present in the reaction furnace.
【００２１】層間化合物形成用気相成長炭素繊維とゲス
ト材料との使用割合は、層間化合物形成用気相成長炭素
繊維とゲスト材料との種類およびそれらの組み合わせに
より相違するので一概に決定することはできないのであ
るが、例えばゲスト材料がハロゲン化金属であるときに
は、通常、層間化合物形成用気相成長炭素繊維１０〜６
０重量％、特に２０〜５０重量％、ハロゲン化金属４０
〜９０重量％、特に５０〜８０重量％である。The use ratio of the vapor-grown carbon fiber for forming an intercalation compound and the guest material differs depending on the kind of the vapor-grown carbon fiber for forming an intercalation compound and the guest material and a combination thereof, and therefore cannot be determined unconditionally. Although it is not possible, for example, when the guest material is a metal halide, the vapor-grown carbon fibers 10 to 6 for forming an intercalation compound are usually used.
0% by weight, especially 20 to 50% by weight, metal halide 40
-90% by weight, especially 50-80% by weight.
【００２２】[0022]
【実施例】以下にこの発明の実施例を示す。この発明は
以下の実施例に限定されるものではなく、この発明の要
旨の範囲内において適宜に変更することができるのでは
いうまでもない。EXAMPLES Examples of the present invention will be shown below. It is needless to say that the present invention is not limited to the following examples and can be appropriately modified within the scope of the gist of the present invention.
【００２３】（実施例１）平均直径が１μｍ，平均長さ
が１２６μｍ、平均アスペクト比が１２６の気相成長炭
素繊維をアルゴンガス雰囲気中で２，８００℃で３０分
間黒鉛化処理した。その後に、高速気流中での衝撃処理
を行うハイブリダイザー（ＮＨＳ−１、（株）奈良機械
製作所製）を用い、７，０００ｒｐｍ（周速８７．５ｍ
／ｓ）にて２分間衝撃処理をした。処理後得られた繊維
は、平均直径が１μｍ、平均長さが２３μｍ、アスペク
ト比２３、ｄ002 が３．３６２Å、Ｌｃが１，０００Å
以上であった。Example 1 A vapor grown carbon fiber having an average diameter of 1 μm, an average length of 126 μm and an average aspect ratio of 126 was graphitized at 2,800 ° C. for 30 minutes in an argon gas atmosphere. After that, a hybridizer (NHS-1, manufactured by Nara Machinery Co., Ltd.) that performs impact treatment in a high-speed airflow was used and 7,000 rpm (peripheral speed 87.5 m
/ S) for 2 minutes. The fibers obtained after the treatment have an average diameter of 1 μm, an average length of 23 μm, an aspect ratio of 23, a d 002 of 3.362Å, and an Lc of 1,000 Å.
That was all.
【００２４】その後、図１に示すＧＩＣ製造装置におい
て、セラミック製の耐熱腐食性筒体３内の仕切り板１１
の上にホスト材料として上記記載の黒鉛化気相成長炭素
繊維５００ｇを載せるとともに、仕切り版１１の下にゲ
スト材料として約１．５ｋｇの無水塩化第二鉄分を収納
し、加熱炉１の蓋２を閉じて真空排気した。Thereafter, in the GIC manufacturing apparatus shown in FIG. 1, the partition plate 11 in the ceramic heat-resistant and corrosion-resistant cylindrical body 3 is used.
500 g of the graphitized vapor-grown carbon fiber described above is placed as a host material on the top, and about 1.5 kg of anhydrous ferric chloride is stored as a guest material under the partition plate 11, and the lid 2 of the heating furnace 1 is placed. Was closed and evacuated.
【００２５】続いて加熱炉１内に塩素ガスを４００Ｔｏ
ｒｒまで導入したのち、耐熱耐腐食性筒体３の蓋部材４
をロッド５で閉め、加熱炉１内を真空排気し、その後、
加熱炉１内を空気で満たした。Subsequently, the heating furnace 1 was filled with chlorine gas at 400 To
After introducing up to rr, the lid member 4 of the heat and corrosion resistant cylinder 3
Is closed with a rod 5, the inside of the heating furnace 1 is evacuated, and then
The heating furnace 1 was filled with air.
【００２６】次に、加熱炉１内を３５０℃に２４時間加
熱したのち、変性黒鉛化気相成長炭素繊維を取り出した
ところ、この繊維の重量が１．６５ｋｇであり、Ｘ線回
折からｄ002 は９．５５Åを示し、第一ステージの塩化
第二鉄層間化合物になっていた。Next, after heating the inside of the heating furnace 1 to 350 ° C. for 24 hours, the modified graphitized vapor grown carbon fiber was taken out. The weight of this fiber was 1.65 kg, and d 002 was obtained by X-ray diffraction. Was 9.55Å, which was a ferric chloride intercalation compound in the first stage.
【００２７】なお、図１において、加熱炉１は、加熱炉
本体の開口部に蓋２を開閉自在に取り付けてなる。加熱
炉本体の内部には、一端が開口した耐熱耐腐食性筒体３
が加熱炉本体の内壁から所定間隔を設けて収納される。
この耐熱耐腐食性筒体３の開口部には蓋部材４が装着さ
れる。この蓋体４にはロッド５が装着される。そのロッ
ド５は蓋２を貫通して加熱炉本体の外部に突き出てい
る。このロッド５は図示しない駆動装置により前後動可
能になっている。したがって、このロッド５を前後動さ
せると、このロッド５の先端部に装着された蓋部材４が
前記耐熱耐腐食性筒体３の開口部を閉鎖し、あるいは解
放する。したがって、耐熱耐腐食性筒体３の開口部は、
加熱炉本体の開口部が密閉されている状態でも、外部か
ら密閉開放することができる。なお、蓋２の外面とロッ
ド５との間にはＯリング６が設けられている。In FIG. 1, the heating furnace 1 has a lid 2 which is openably and closably attached to the opening of the heating furnace body. Inside the heating furnace body, a heat-resistant and corrosion-resistant cylindrical body 3 with one end open
Are housed at a predetermined distance from the inner wall of the heating furnace body.
A lid member 4 is attached to the opening of the heat and corrosion resistant cylinder 3. A rod 5 is attached to the lid 4. The rod 5 penetrates the lid 2 and projects to the outside of the furnace body. The rod 5 can be moved back and forth by a driving device (not shown). Therefore, when the rod 5 is moved back and forth, the lid member 4 attached to the tip of the rod 5 closes or releases the opening of the heat and corrosion resistant tubular body 3. Therefore, the opening of the heat and corrosion resistant cylinder 3 is
Even when the opening of the heating furnace body is sealed, it can be sealed and opened from the outside. An O-ring 6 is provided between the outer surface of the lid 2 and the rod 5.
【００２８】また、それぞれ蓋２を閉じた際の加熱炉１
内の気密を保持す目的で加熱炉本体の開口端面と蓋２と
の間には蓋２の局部冷却が可能であるため、ゴム等の一
般的なシール部材１６が設けられ、耐熱耐腐食性筒体３
の開口端面と蓋部材４との間にはたとえば断熱性グラフ
ァイトのようなシール部材１７が設けられている。加熱
炉本体の内面は、耐熱性および気密性の材料、たとえば
ステンレス７で構成され、その外側はヒータ８および断
熱材料９で構成され、この断熱材料９の外面はカバー１
０で覆われている。Further, the heating furnace 1 when the lid 2 is closed
Since the lid 2 can be locally cooled between the opening end surface of the heating furnace main body and the lid 2 for the purpose of maintaining the airtightness inside, a general sealing member 16 such as rubber is provided, and heat resistance and corrosion resistance are provided. Cylinder 3
A seal member 17 made of, for example, heat-insulating graphite is provided between the open end surface of the lid member 4 and the lid member 4. The inner surface of the heating furnace body is made of a heat-resistant and airtight material, for example, stainless steel 7, the outer side thereof is made of a heater 8 and a heat insulating material 9, and the outer surface of this heat insulating material 9 is the cover 1.
It is covered with 0.
【００２９】断熱材料９としては公知のもので良く、た
とえばガラス綿、レンガ、微粉鉱物などがある。耐熱耐
腐食性筒体３は高度の耐腐食性材料、たとえば高温の塩
素系ガスにも耐えるようセラミックス、ガラス、および
これらでライニングされた金属などの材料で構成され、
内部は多孔を有する仕切り板１１で画され、その上部に
ホスト材料としての炭素材料１２を、またその下部にゲ
スト材料１３を収納できるようになっている。Any known material may be used as the heat insulating material 9, and examples thereof include glass cotton, brick, and fine powder minerals. The heat and corrosion resistant cylinder 3 is made of a highly corrosive resistant material, for example, a material such as ceramics, glass, and a metal lined with these so as to withstand high temperature chlorine-based gas,
The interior is defined by a partition plate 11 having porosity, and a carbon material 12 as a host material can be accommodated in the upper part thereof and a guest material 13 can be accommodated in the lower part thereof.
【００３０】加熱炉本体の内部空間は、蓋２を貫通する
パイプ１４を介して排気手段およびガス導入手段（図示
せず）と連絡され、パイプ１４には蓋２に近い箇所に圧
力計１５および温度計（図示せず）が取り付けられてい
る。なお、前記パイプ１４は、蓋２を貫通していなくて
も加熱炉本体を貫通していても良い。耐熱耐腐食性筒体
３は、通常加熱炉本体に固定されているが、取り外しも
可能である。The internal space of the heating furnace body is connected to an exhaust means and a gas introduction means (not shown) through a pipe 14 penetrating the lid 2, and the pipe 14 has a pressure gauge 15 and a gas gauge 15 at a position near the lid 2. A thermometer (not shown) is attached. The pipe 14 may not penetrate the lid 2 but may penetrate the heating furnace main body. The heat-resistant and corrosion-resistant cylindrical body 3 is usually fixed to the heating furnace body, but can be removed.
【００３１】（比較例）平均直径が１μｍ、平均長さが
１２６μｍ、平均アスペクト比が１２６の気相成長炭素
繊維をハイブリダイザー、ＮＨＳ−１、（株）奈良機械
製作所製）で、７，０００ｒｐｍ（周速８７．５ｍ／
ｓ）にて２分間処理した後、アルゴンガス雰囲気中で
２，８００℃、３０分間黒鉛化処理をした。Comparative Example A vapor-grown carbon fiber having an average diameter of 1 μm, an average length of 126 μm, and an average aspect ratio of 126 was used at 7,000 rpm with a hybridizer, NHS-1, manufactured by Nara Machinery Co., Ltd. (Peripheral speed 87.5m /
s) for 2 minutes, and then graphitized at 2,800 ° C. for 30 minutes in an argon gas atmosphere.
【００３２】得られた繊維は、平均直径が１μｍ、平均
長さが２５μｍ、アスペクト比が２５、ｄ002 が３．３
６２Å、Ｌｃが１，０００Å以上であった。The obtained fiber has an average diameter of 1 μm, an average length of 25 μm, an aspect ratio of 25 and a d 002 of 3.3.
62Å, Lc was 1,000Å or more.
【００３３】この繊維を用い、実施例１と同様に実験を
行なったところ、得られた変性黒鉛化気相成長炭素繊維
は、Ｘ線回折からｄ002 は９．５５Åを示し、第一ステ
ージの塩化第二鉄層間化合物になっていることが確認さ
れたが、その重量は０．９５ｋｇであった。Using this fiber, an experiment was conducted in the same manner as in Example 1. As a result, the modified graphitized vapor-grown carbon fiber obtained had a d 002 of 9.55Å as determined by X-ray diffraction. It was confirmed to be a ferric chloride intercalation compound, but its weight was 0.95 kg.
【００３４】[0034]
【発明の効果】この発明によると、ゲスト材料を受け入
れて迅速に層間化合物を形成することのできる層間化合
物形成用に好適な黒鉛化気相成長炭素繊維及びその製造
方法を提供することができる。According to the present invention, it is possible to provide a graphitized vapor-grown carbon fiber suitable for forming an intercalation compound capable of receiving a guest material and rapidly forming an intercalation compound, and a method for producing the same.
【図１】この発明の層間化合物の製造装置の一例を示す
説明図である。FIG. 1 is an explanatory view showing an example of an apparatus for producing an intercalation compound of the present invention.
１ 加熱炉 ２ 蓋体 ３ 反応炉 ４ 蓋体 １２ ホスト材料としての層間化合物形成用気相成長炭
素繊維 １３ ゲスト材料 １４ ガス置換手段のパイプDESCRIPTION OF SYMBOLS 1 Heating furnace 2 Lid body 3 Reactor 4 Lid body 12 Vapor-grown carbon fiber for forming intercalation compound as host material 13 Guest material 14 Pipe of gas replacement means
Claims (3)
した後に粉砕してなることを特徴とする層間化合物形成
用黒鉛化気相成長炭素繊維。1. A graphitized vapor-grown carbon fiber for forming an intercalation compound, characterized in that the vapor-grown carbon fiber is substantially graphitized and then pulverized.
以下である前記請求項１に記載の層間化合物形成用黒鉛
化気相成長炭素繊維。2. A diameter of 5 μm or less and an aspect ratio of 50.
The graphitized vapor-grown carbon fiber for forming an intercalation compound according to claim 1, wherein:
した後に粉砕することを特徴とする層間化合物形成用黒
鉛化気相成長炭素繊維の製造方法。3. A method for producing a graphitized vapor grown carbon fiber for forming an intercalation compound, which comprises substantially graphitizing the vapor grown carbon fiber and then pulverizing the same.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23318492A JPH0681218A (en) | 1992-09-01 | 1992-09-01 | Graphitized vapor-grown carbon fiber for forming interlaminar compound and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23318492A JPH0681218A (en) | 1992-09-01 | 1992-09-01 | Graphitized vapor-grown carbon fiber for forming interlaminar compound and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0681218A true JPH0681218A (en) | 1994-03-22 |
Family
ID=16951057
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23318492A Pending JPH0681218A (en) | 1992-09-01 | 1992-09-01 | Graphitized vapor-grown carbon fiber for forming interlaminar compound and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0681218A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005070535A1 (en) * | 2004-01-27 | 2005-08-04 | Showa Denko K.K. | Catalyst support and fuel cell using same |
| US7150840B2 (en) | 2002-08-29 | 2006-12-19 | Showa Denko K.K. | Graphite fine carbon fiber, and production method and use thereof |
| US7749935B2 (en) | 2004-01-27 | 2010-07-06 | Showa Denko K.K. | Catalyst carrier and fuel cell using the same |
-
1992
- 1992-09-01 JP JP23318492A patent/JPH0681218A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7150840B2 (en) | 2002-08-29 | 2006-12-19 | Showa Denko K.K. | Graphite fine carbon fiber, and production method and use thereof |
| WO2005070535A1 (en) * | 2004-01-27 | 2005-08-04 | Showa Denko K.K. | Catalyst support and fuel cell using same |
| KR100833154B1 (en) * | 2004-01-27 | 2008-05-28 | 쇼와 덴코 가부시키가이샤 | Catalyst support and fuel cell using same |
| US7749935B2 (en) | 2004-01-27 | 2010-07-06 | Showa Denko K.K. | Catalyst carrier and fuel cell using the same |
| US7919427B2 (en) | 2004-01-27 | 2011-04-05 | Showa Denko K.K. | Catalyst carrier and fuel cell using the same |
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