JP2001279305A - Iron-based nanometer scale acicular body and its production method - Google Patents
Iron-based nanometer scale acicular body and its production methodInfo
- Publication number
- JP2001279305A JP2001279305A JP2000093848A JP2000093848A JP2001279305A JP 2001279305 A JP2001279305 A JP 2001279305A JP 2000093848 A JP2000093848 A JP 2000093848A JP 2000093848 A JP2000093848 A JP 2000093848A JP 2001279305 A JP2001279305 A JP 2001279305A
- Authority
- JP
- Japan
- Prior art keywords
- iron
- based nanometer
- scale
- needle
- scale needle
- 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 150000002506 iron compounds Chemical class 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 239000011651 chromium Substances 0.000 claims description 4
- 150000002902 organometallic compounds Chemical class 0.000 claims description 4
- -1 iron halides Chemical class 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 239000011347 resin Substances 0.000 abstract description 24
- 229920005989 resin Polymers 0.000 abstract description 24
- 239000000463 material Substances 0.000 abstract description 15
- 239000004020 conductor Substances 0.000 abstract description 13
- 239000003054 catalyst Substances 0.000 abstract description 6
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 150000002505 iron Chemical class 0.000 abstract description 2
- 239000012808 vapor phase Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 19
- 239000013078 crystal Substances 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- WSSMOXHYUFMBLS-UHFFFAOYSA-L iron dichloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Fe+2] WSSMOXHYUFMBLS-UHFFFAOYSA-L 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 239000012778 molding material Substances 0.000 description 2
- ACMIJDVJWLMBCX-PXAZEXFGSA-N 4-[(3ar,6ar)-2,3,3a,4,6,6a-hexahydro-1h-pyrrolo[2,3-c]pyrrol-5-yl]-6-fluoro-n-methyl-2-(2-methylpyrimidin-5-yl)oxy-9h-pyrimido[4,5-b]indol-8-amine Chemical compound CNC1=CC(F)=CC(C2=C(N3C[C@@H]4NCC[C@@H]4C3)N=3)=C1NC2=NC=3OC1=CN=C(C)N=C1 ACMIJDVJWLMBCX-PXAZEXFGSA-N 0.000 description 1
- YSQCCTFSTWDLFG-UHFFFAOYSA-L C1(C=CC=C1)[Fe](Cl)Cl Chemical compound C1(C=CC=C1)[Fe](Cl)Cl YSQCCTFSTWDLFG-UHFFFAOYSA-L 0.000 description 1
- 101100219325 Phaseolus vulgaris BA13 gene Proteins 0.000 description 1
- QERCSHGKUOHOSS-UHFFFAOYSA-L S(=O)(=O)([O-])[O-].[Fe+2].[O-2].[Fe+2] Chemical compound S(=O)(=O)([O-])[O-].[Fe+2].[O-2].[Fe+2] QERCSHGKUOHOSS-UHFFFAOYSA-L 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003738 black carbon Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 description 1
- 150000002816 nickel compounds Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、針状体、特に、ナ
ノメートルスケールの鉄系針状体に関する。The present invention relates to needles, and more particularly, to a nanometer-scale iron-based needle.
【０００２】[0002]
【従来の技術とその課題】ＩＣトレーをはじめとする各
種の電子部品用途に用いられる樹脂成形品は、帯電に起
因する放電が電子部品を破損してしまうのを防止するた
めに、帯電防止材により導電性を付与されている場合が
多い。ここで用いられる帯電防止材は、例えば炭素繊維
や鉄粉などの導電性材料であり、樹脂成形品中において
互いに接触し合うことにより導電性の通路を形成し、樹
脂成形品に対して導電性を付与している。従って、導電
性材料は、樹脂成形品中において互いに有効に接触し合
える程度の十分な量が含まれていない限り、樹脂成形品
に導電性を付与するのは困難である。2. Description of the Related Art A resin molded product used for various electronic parts such as an IC tray is provided with an antistatic material in order to prevent a discharge caused by charging from damaging the electronic parts. In many cases, conductivity is given by The antistatic material used here is, for example, a conductive material such as carbon fiber or iron powder, and forms a conductive path by being in contact with each other in a resin molded product, thereby forming a conductive material on the resin molded product. Has been granted. Therefore, it is difficult to impart conductivity to the resin molded product unless the conductive material contains a sufficient amount of the conductive material to be able to effectively contact each other.
【０００３】ところが、樹脂成形品は、多量の導電性材
料を含む場合、強度等の各種特性が損なわれる場合があ
る。また、多量の導電性材料を含む樹脂成形品は、全体
に導電性材料の色彩が強く反映され易く、着色材等を用
いて所望の色彩を自由に付与するのは困難な場合が多
い。例えば、黒色の炭素繊維を多く含む樹脂成形品は、
炭素繊維による特有の黒色を呈することになるため、着
色材を同時に含んでいても、当該着色材の色彩は反映さ
れにくい。このため、樹脂成形品の技術分野において
は、少量の添加で効果的に導電性を付与することができ
る導電性材料が求められている。However, when a resin molded product contains a large amount of a conductive material, various properties such as strength may be impaired. In addition, a resin molded product containing a large amount of a conductive material tends to strongly reflect the color of the conductive material as a whole, and it is often difficult to freely impart a desired color using a coloring material or the like. For example, a resin molded product containing a large amount of black carbon fiber,
Since the carbon material exhibits a unique black color, the color of the colorant is hardly reflected even when the colorant is included at the same time. For this reason, in the technical field of resin molded products, a conductive material that can effectively impart conductivity with a small amount of addition is required.
【０００４】本発明の目的は、例えば樹脂成形品用の導
電性材料等として有用な、新規な鉄系材料を実現するこ
とにある。An object of the present invention is to realize a novel iron-based material useful as, for example, a conductive material for a resin molded product.
【０００５】[0005]
【課題を解決するための手段】本発明の鉄系ナノメート
ルスケール針状体は、実質的に鉄元素からなる針状体で
あって、太さが１，０００ｎｍ未満である。この鉄系ナ
ノメートルスケール針状体は、好ましくは、太さが１０
０ｎｍ以下である。また、この鉄系ナノメートルスケー
ル針状体は、例えば、アスペクト比が少なくとも５であ
る。さらに、この鉄系ナノメートルスケール針状体は、
例えば、実質的に直線状である。さらに、この鉄系ナノ
メートルスケール針状体は、例えば、鉄元素以外の異種
金属元素を含有している。ここで、異種金属元素は、例
えば、クロムおよびニッケルのうちの少なくとも１種で
ある。The iron-based nanometer-scale needle-shaped body of the present invention is a needle-shaped body substantially composed of iron element and has a thickness of less than 1,000 nm. The iron-based nanometer-scale needle-shaped body preferably has a thickness of 10
0 nm or less. The iron-based nanometer-scale acicular body has, for example, an aspect ratio of at least 5. Furthermore, this iron-based nanometer-scale needle
For example, it is substantially straight. Further, the iron-based nanometer-scale needle-shaped body contains, for example, a different metal element other than the iron element. Here, the dissimilar metal element is, for example, at least one of chromium and nickel.
【０００６】本発明に係る鉄系ナノメートルスケール針
状体の製造方法は、鉄化合物を気相において還元する工
程を含んでいる。ここで、鉄化合物は、例えば２価の鉄
の化合物であり、この２価の鉄の化合物は、例えば、２
価の鉄のハロゲン化物および２価の鉄を要素とする有機
金属化合物からなる群から選択された少なくとも１種で
ある。また、この製造方法において、気相は、例えば還
元剤を含んでいる。ここで用いられる還元剤は、例えば
水素である。さらに、この製造方法では、通常、気相の
温度を２００〜１，５００℃に設定している。The method for producing an iron-based nanometer-scale needle according to the present invention includes a step of reducing an iron compound in a gas phase. Here, the iron compound is, for example, a divalent iron compound.
It is at least one selected from the group consisting of halides of divalent iron and organometallic compounds containing divalent iron as an element. In this manufacturing method, the gas phase contains, for example, a reducing agent. The reducing agent used here is, for example, hydrogen. Further, in this manufacturing method, the temperature of the gas phase is usually set at 200 to 1,500 ° C.
【０００７】[0007]
【発明の実施の形態】本発明の鉄系ナノメートルスケー
ル針状体は、実質的に鉄元素からなる新規な針状の極細
材料であり、鉄化合物を気相において還元することによ
り製造され得る。BEST MODE FOR CARRYING OUT THE INVENTION The iron-based nanometer-scale needle-shaped material of the present invention is a novel needle-shaped ultrafine material substantially composed of iron element, and can be produced by reducing an iron compound in a gas phase. .
【０００８】本発明の鉄系ナノメートルスケール針状体
を製造する場合に用いられる鉄化合物は、公知の各種の
鉄化合物であって特に限定されるものではないが、例え
ば、塩化鉄（ＦｅＣｌ2）や塩化鉄４水和物（ＦｅＣｌ2
・４Ｈ2Ｏ）等の２価の鉄のハロゲン化物、フェロセ
ン，鉄アセチルアセトナート，鉄ベンゾイルアセトナー
ト，鉄ペンタカルボニルおよびジクロロペンタジエニル
鉄等の鉄を要素とする有機金属化合物、硫酸鉄並びに酸
化鉄を挙げることができる。このうち、２価の鉄のハロ
ゲン化物、及びフェロセン等の２価の鉄を要素とする有
機金属化合物等の、２価の鉄の化合物を用いるのが好ま
しい。このような鉄化合物は、それぞれ単独で用いられ
てもよいし、２種以上のものが併用されてもよい。The iron compound used for producing the iron-based nanometer-scale needles of the present invention is not particularly limited, and is not particularly limited, and may be, for example, iron chloride (FeCl 2). ) Or iron chloride tetrahydrate (FeCl 2
· 4H 2 O) 2-valent halides of iron such as ferrocene, iron acetylacetonate, iron benzoylacetonate toner DOO, organometallic compounds and iron pentacarbonyl and dichloro cyclopentadienyl iron elements such as iron, and iron sulfate Iron oxide may be mentioned. Of these, it is preferable to use divalent iron compounds such as divalent iron halides and organometallic compounds containing divalent iron such as ferrocene. Such iron compounds may be used alone or in combination of two or more.
【０００９】上述の鉄化合物を気相で還元する場合に
は、通常、加熱炉中において鉄化合物を気化させ、当該
気化された鉄化合物を還元性雰囲気下で熱処理する。こ
の際、気相の温度、すなわち、加熱炉内の温度は、通
常、２００〜１，５００℃に設定するのが好ましく、４
００〜８００℃に設定するのがより好ましく、５００〜
６００℃に設定するのがさらに好ましい。この温度が２
００℃未満の場合は、目的とする鉄系ナノメートルスケ
ール針状体が得られにくい場合がある。逆に、１，５０
０℃を超えると、本発明の鉄系ナノメートルスケール針
状体の製造コストが高まり、不経済である。When the above-mentioned iron compound is reduced in the gas phase, usually, the iron compound is vaporized in a heating furnace, and the vaporized iron compound is heat-treated in a reducing atmosphere. At this time, the temperature of the gas phase, that is, the temperature in the heating furnace is usually preferably set to 200 to 1,500 ° C.
It is more preferable to set the temperature to 00 to 800 ° C,
More preferably, the temperature is set to 600 ° C. This temperature is 2
If the temperature is lower than 00 ° C., it may be difficult to obtain a desired iron-based nanometer-scale needle-shaped body. Conversely, 1,50
If the temperature exceeds 0 ° C., the production cost of the iron-based nanometer-scale needles of the present invention increases, which is uneconomical.
【００１０】また、熱処理時間、即ち鉄化合物の還元に
要する時間は、使用する鉄化合物の種類や量などにより
異なるため、特に限定されるものではないが、通常、１
〜１，０００分程度に設定するのが好ましく、５〜１２
０分程度に設定するのがより好ましい。The heat treatment time, that is, the time required for reducing the iron compound, varies depending on the type and amount of the iron compound used, and is not particularly limited.
It is preferably set to about 1,000 minutes, and 5 to 12 minutes.
It is more preferable to set the time to about 0 minutes.
【００１１】なお、加熱炉内は、還元性雰囲気に設定さ
れる前の状態において、真空状態（脱気状態）または窒
素やヘリウム等の不活性ガスを導入した不活性状態に設
定されているのが好ましい。加熱炉内がこのように設定
されていない場合、鉄化合物が気相で還元される前に例
えば酸化等の作用を受けることになるため、目的とする
鉄系ナノメートルスケール針状体が得られない可能性が
ある。The heating furnace is set to a vacuum state (a degassed state) or an inert state in which an inert gas such as nitrogen or helium is introduced before the reducing atmosphere is set. Is preferred. If the inside of the heating furnace is not set in this manner, the iron compound will be subjected to an action such as oxidation before being reduced in the gas phase, so that the desired iron-based nanometer-scale needle-shaped body is obtained. May not be.
【００１２】加熱炉内を還元性雰囲気に設定するために
は、通常、還元剤を用いるのが好ましい。本発明におい
て利用する還元剤としては、水素が好ましい。In order to set the inside of the heating furnace to a reducing atmosphere, it is usually preferable to use a reducing agent. Hydrogen is preferred as the reducing agent used in the present invention.
【００１３】なお、上述の還元剤は、鉄化合物と共に当
初から加熱炉内に導入されていてもよいし、加熱炉内の
温度を高めるに従って加熱炉内に徐々に導入してもよ
い。還元剤の使用量は、鉄化合物を十分に還元できる程
度に設定されていれば、特に限定されるものではない。The above reducing agent may be introduced into the heating furnace together with the iron compound from the beginning, or may be gradually introduced into the heating furnace as the temperature in the heating furnace is increased. The amount of the reducing agent used is not particularly limited as long as it is set to an extent that the iron compound can be sufficiently reduced.
【００１４】本発明の鉄系ナノメートルスケール針状体
は、通常、加熱炉の内壁面等に付着した状態で得られ
る。[0014] The iron-based nanometer-scale acicular body of the present invention is usually obtained in a state of being attached to the inner wall surface of a heating furnace or the like.
【００１５】上述のような製造方法により得られる本発
明の鉄系ナノメートルスケール針状体は、実質的に鉄元
素からなり、通常、円柱状、楕円柱状、三角柱状、四角
柱状または多角柱状等の形状であって極細の針状物、即
ち、太さがナノメートルスケールの針状物である。より
具体的には、太さが１，０００ｎｍ未満、好ましくは１
００ｎｍ以下の針状物である。ここで、“太さ”とは、
針状物が円柱状の場合は直径を、楕円柱状の場合は長径
を、多角柱等の角柱状の場合は最長の対角距離をそれぞ
れ意味している。換言すると、ここでの“太さ”とは、
針状物の長さ方向に対して垂直な面における最大幅を意
味している。The iron-based nanometer-scale needle-shaped body of the present invention obtained by the above-described production method is substantially composed of an iron element, and is usually in the form of a column, an ellipse, a triangle, a square or a polygon. And an ultrafine needle, that is, a needle having a thickness of nanometer scale. More specifically, the thickness is less than 1,000 nm, preferably 1
It is a needle-shaped object having a size of 00 nm or less. Here, "thickness"
When the needle-like object is cylindrical, it means the diameter, when it is elliptical, it means the major axis, and when it is prismatic, such as a polygonal pillar, it means the longest diagonal distance. In other words, "thickness" here means
It means the maximum width in a plane perpendicular to the length direction of the needle.
【００１６】また、本発明の鉄系ナノメートルスケール
針状体は、通常、実質的に直線状のものであり、また、
通常、アスペクト比（長さ／太さ）が少なくとも５、好
ましくは少なくとも１０である。[0016] The iron-based nanometer-scale acicular body of the present invention is generally substantially linear.
Usually, the aspect ratio (length / thickness) is at least 5, preferably at least 10.
【００１７】なお、本発明の鉄系ナノメートルスケール
針状体は、上述の通り、実質的に鉄元素からなるもので
あるが、鉄元素以外の異種金属元素を微量に含んでいて
もよい。また、この異種金属元素は、鉄元素と共に化合
物を形成していてもよい。異種金属元素は、特に限定さ
れるものではないが、例えばクロムまたはニッケルを挙
げることができる。鉄系ナノメートルスケール針状体に
は、複数種類の異種金属元素、例えばクロムとニッケル
とが同時に含まれていてもよい。As described above, the iron-based nanometer-scale acicular body of the present invention is substantially made of an iron element, but may contain a trace amount of a different metal element other than the iron element. Further, the dissimilar metal element may form a compound together with the iron element. The dissimilar metal element is not particularly limited, and examples thereof include chromium and nickel. The iron-based nanometer-scale needle-shaped body may simultaneously contain a plurality of types of different metal elements, for example, chromium and nickel.
【００１８】このような微量の異種金属元素を含む鉄系
ナノメートルスケール針状体は、例えば、上述の製造方
法において、上述の鉄化合物と共に、微量の異種金属化
合物、例えばクロム化合物やニッケル化合物を同時に気
相において還元すると得られる。ここで用いられる異種
金属化合物は、例えば、上述の異種金属元素のハロゲン
化物や有機金属化合物などである。因みに、上述の製造
方法において用いる加熱炉が金属製（例えばステンレス
製）のものである場合、当該加熱炉を構成する金属のコ
ンタミネーションに起因して、微量の異種金属元素を含
む鉄系ナノメートルスケール針状体が生成する場合もあ
る。Such an iron-based nanometer-scale needle containing a trace amount of a foreign metal element can be obtained by, for example, using the above-mentioned production method together with a trace amount of a foreign metal compound such as a chromium compound or a nickel compound. It is obtained by reduction in the gas phase at the same time. The different metal compound used here is, for example, a halide or an organometal compound of the above-described different metal element. Incidentally, when the heating furnace used in the above-mentioned manufacturing method is made of metal (for example, stainless steel), an iron-based nanometer containing a trace amount of a different metal element due to contamination of the metal constituting the heating furnace. A scale needle may be formed.
【００１９】因みに、本発明の鉄系ナノメートルスケー
ル針状体は、上述の通り実質的に鉄元素からなるため、
微量の異種金属元素を含む場合であっても、磁石に吸着
され得る。Incidentally, since the iron-based nanometer-scale acicular body of the present invention is substantially composed of iron as described above,
Even when a trace amount of a different metal element is contained, it can be adsorbed by the magnet.
【００２０】本発明の鉄系ナノメートルスケール針状体
は、各種の技術分野において有効に利用することができ
る。The iron-based nanometer-scale needles of the present invention can be effectively used in various technical fields.
【００２１】例えば、本発明の鉄系ナノメートルスケー
ル針状体は、樹脂成形体に対して導電性を付与するため
の導電性材料として利用することができる。この場合
は、樹脂材料に対して本発明の針状体を添加して成形材
料を調製する。そして、当該成形材料を所望の形状に成
形すると、導電性を有する樹脂成形体が得られる。ここ
で、本発明の針状体は、これまでにない極細の針状体で
あるため、樹脂材料に対して少量添加しただけでも、樹
脂材料中で相互に点接触する確率が高まることになる。
したがって、本発明の針状体は、樹脂材料に対する添加
量を抑制しながら（即ち、少量に設定しつつ）、樹脂成
形体に対して効果的な導電性を付与することができる。
また、本発明の針状体は、樹脂材料に対して少量添加す
るだけで十分に樹脂成形体の導電性を高め得るため、そ
の色彩は樹脂成形体に反映されにくい。したがって、本
発明の針状体を各種の着色材と共に樹脂材料に添加すれ
ば、これまでの導電性材料では達成が困難であった樹脂
成形体、即ち、所要の導電性を示し、しかも所望の色彩
に着色された樹脂成形体を実現することができる。For example, the iron-based nanometer-scale needle-shaped body of the present invention can be used as a conductive material for imparting conductivity to a resin molded body. In this case, the molding material is prepared by adding the needle-shaped body of the present invention to the resin material. Then, when the molding material is molded into a desired shape, a resin molded body having conductivity is obtained. Here, since the needle-shaped body of the present invention is an unprecedented ultra-fine needle-shaped body, even if a small amount is added to the resin material, the probability of point contact with each other in the resin material is increased. .
Therefore, the needle-shaped body of the present invention can impart effective conductivity to the resin molded body while suppressing the amount of addition to the resin material (that is, while setting the amount to a small amount).
Further, the needle-shaped body of the present invention can sufficiently enhance the conductivity of the resin molded body by adding a small amount to the resin material, and therefore, the color is hardly reflected on the resin molded body. Therefore, if the needle-shaped body of the present invention is added to a resin material together with various coloring materials, a resin molded body, which has been difficult to achieve with conventional conductive materials, that is, exhibits required conductivity, and has a desired conductivity. A colored resin molded product can be realized.
【００２２】また、本発明の鉄系ナノメートルスケール
針状体は、実質的に鉄元素からなるために従来の鉄系材
料と同じく各種の触媒として利用可能であるが、極細の
針状体である点において特徴的であるため、粉状等の鉄
系触媒に比べて高い触媒活性を発揮し得る。このため、
例えば、各種の有機合成反応用の触媒として本発明の針
状体を用いると、目的とする化合物を高収率で得ること
ができるものと考えられる。特に、本発明の針状体は、
メタンから水素ガスを製造するためのシフト反応用の触
媒として用いられた場合、効率的に水素ガスを製造する
ことができる点で有利である。The iron-based nanometer-scale needles of the present invention can be used as various catalysts like conventional iron-based materials because they are substantially composed of iron element. Since it is characteristic in a certain point, it can exhibit higher catalytic activity than a powdery iron-based catalyst. For this reason,
For example, it is considered that the target compound can be obtained in high yield by using the needle-shaped body of the present invention as a catalyst for various organic synthesis reactions. In particular, the needle-shaped body of the present invention,
When used as a catalyst for a shift reaction for producing hydrogen gas from methane, it is advantageous in that hydrogen gas can be produced efficiently.
【００２３】さらに、本発明の鉄系ナノメートルスケー
ル針状体は、実質的に鉄元素からなるため、従来の鉄系
材料と同じく磁気記録媒体用の磁性材料としての用途も
期待することができる。因みに、本発明の針状体は、極
細の針状体である点において特徴的であり、そのような
特徴のため異方性が大きいので、鉄粉等の従来の磁性材
料に比べて記録性能の高い磁気記録媒体を実現する上で
有用と考えられる。Further, since the iron-based nanometer-scale needle-shaped body of the present invention is substantially composed of iron element, it can be expected to be used as a magnetic material for a magnetic recording medium like a conventional iron-based material. . Incidentally, the needle-shaped body of the present invention is characteristic in that it is an ultra-fine needle-shaped body. It is considered to be useful in realizing a magnetic recording medium having a high density.
【００２４】なお、上述の各種の利用方法は、単なる例
示であり、本発明の鉄系ナノメートルスケール針状体
は、その他の技術分野における用途展開も期待すること
ができる。The above-mentioned various uses are merely examples, and the use of the iron-based nanometer-scale needles of the present invention in other technical fields can be expected.
【００２５】[0025]
【実施例】実施例 ０．４ｇの塩化鉄４水和物（ＦｅＣｌ2・４Ｈ2Ｏ）をニ
ッケル製ボートに設置し、加熱炉内にこのボートを配置
した。加熱炉の内部を真空脱気した後、加熱炉を作動さ
せ、内部温度が４００℃に到達した時点で加熱炉内に２
０ｃｃ／分の割合で水素を導入した。これにより、加熱
炉の内部を水素雰囲気、すなわち還元性雰囲気に設定し
た。この状態で加熱炉の内部温度を更に６００℃まで高
め、当該温度において３０分間、塩化鉄４水和物を気相
において還元した。この際、加熱炉内の圧力は５００Ｔ
ｏｒｒであった。EXAMPLE Example 0.4 g of iron chloride tetrahydrate (FeCl 2 .4H 2 O) was placed in a nickel boat, and this boat was placed in a heating furnace. After the inside of the heating furnace was degassed by vacuum, the heating furnace was operated. When the internal temperature reached 400 ° C., 2
Hydrogen was introduced at a rate of 0 cc / min. Thus, the inside of the heating furnace was set to a hydrogen atmosphere, that is, a reducing atmosphere. In this state, the internal temperature of the heating furnace was further increased to 600 ° C., and iron chloride tetrahydrate was reduced in the gas phase at the temperature for 30 minutes. At this time, the pressure in the heating furnace was 500 T
orr.
【００２６】還元処理後、加熱炉を常温まで冷却し、そ
の内部を観察したところ、針状の結晶が多数生成してい
ることが確認された。この結晶は、電子線回折法に従っ
て分析した結果、実質的に鉄元素からなるものであるこ
とが確認され、また、磁石にも吸着された。また、当該
結晶の形態は、透過型電子顕微鏡（ＴＥＭ）を用いて観
察した結果、平均太さが５０ｎｍ、平均長さが３μｍの
柱状（アスペクト比＝６０）であることが確認された。
参考のため、ここで得られた針状の結晶のＴＥＭ写真を
図１に示す。After the reduction treatment, the heating furnace was cooled to room temperature, and the inside thereof was observed. As a result, it was confirmed that a large number of needle-like crystals had been formed. As a result of analyzing this crystal according to the electron beam diffraction method, it was confirmed that the crystal was substantially composed of an iron element, and was also adsorbed to a magnet. In addition, as a result of observing the form of the crystal using a transmission electron microscope (TEM), it was confirmed that the crystal had a columnar shape (aspect ratio = 60) having an average thickness of 50 nm and an average length of 3 μm.
For reference, FIG. 1 shows a TEM photograph of the needle-like crystals obtained here.
【００２７】[0027]
【発明の効果】本発明によれば、例えば、樹脂成形体に
対して導電性を付与するための導電性材料、触媒および
磁性材料等として有用な、新規な鉄系材料を提供するこ
とができる。According to the present invention, for example, a novel iron-based material useful as a conductive material, a catalyst, a magnetic material, and the like for imparting conductivity to a resin molded article can be provided. .
【図１】実施例で得られた針状の結晶の透過型電子顕微
鏡写真。FIG. 1 is a transmission electron micrograph of a needle-like crystal obtained in an example.
フロントページの続き (72)発明者 西田 亮一 大阪府大阪市中央区平野町四丁目１番２号 大阪瓦斯株式会社内 (72)発明者 川瀬 昇 京都府京都市下京区中堂寺南町17 株式会 社関西新技術研究所内 (72)発明者 松井 丈雄 京都府京都市下京区中堂寺南町17 株式会 社関西新技術研究所内 Ｆターム(参考） 4G077 AA04 BA01 DB28 HA20 4J002 AA001 DA086 FD116 GQ02 4K017 AA02 BA06 BB04 BB06 CA02 DA01 EH01 EH15 FB03 FB06 4K018 BA13 BB01 BB05 Continued on the front page (72) Inventor Ryoichi Nishida 4-1-2, Hirano-cho, Chuo-ku, Osaka City, Osaka Prefecture Inside Osaka Gas Co., Ltd. Inside the Kansai New Technology Research Institute (72) Inventor Takeo Matsui 17 Nakadoji Minamicho, Shimogyo-ku, Kyoto, Kyoto F Kansai New Technology Research Laboratory F-term (reference) 4G077 AA04 BA01 DB28 HA20 4J002 AA001 DA086 FD116 GQ02 4K017 AA02 BA06 BB04 BB06 CA02 DA01 EH01 EH15 FB03 FB06 4K018 BA13 BB01 BB05
Claims (12)
太さが１，０００ｎｍ未満である、鉄系ナノメートルス
ケール針状体。1. A needle-like body substantially composed of an iron element,
An iron-based nanometer-scale needle having a thickness of less than 1,000 nm.
１に記載の鉄系ナノメートルスケール針状体。2. The iron-based nanometer-scale needle according to claim 1, wherein the thickness is 100 nm or less.
項１または２に記載の鉄系ナノメートルスケール針状
体。3. An iron-based nanometer-scale needle according to claim 1 or 2, wherein the aspect ratio is at least 5.
は３に記載の鉄系ナノメートルスケール針状体。4. The iron-based nanometer-scale needle according to claim 1, which is substantially linear.
いる、請求項１、２、３または４に記載の鉄系ナノメー
トルスケール針状体。5. The iron-based nanometer-scale needle-shaped body according to claim 1, containing a different metal element other than the iron element.
のうちの少なくとも１種である、請求項５に記載の鉄系
ナノメートルスケール針状体。6. The iron-based nanometer-scale needle according to claim 5, wherein the dissimilar metal element is at least one of chromium and nickel.
む、鉄系ナノメートルスケール針状体の製造方法。7. A method for producing an iron-based nanometer-scale needle-like body, comprising a step of reducing an iron compound in a gas phase.
請求項７に記載の鉄系ナノメートルスケール針状体の製
造方法。8. The iron compound is a divalent iron compound,
A method for producing an iron-based nanometer-scale needle according to claim 7.
ン化物および２価の鉄を要素とする有機金属化合物から
なる群から選択された少なくとも１種である、請求項８
に記載の鉄系ナノメートルスケール針状体の製造方法。9. The divalent iron compound is at least one selected from the group consisting of divalent iron halides and organometallic compounds containing divalent iron as an element.
3. The method for producing an iron-based nanometer-scale needle-like body according to item 1.
７、８または９に記載の鉄系ナノメートルスケール針状
体の製造方法。10. The method for producing an iron-based nanometer-scale needle according to claim 7, wherein the gas phase contains a reducing agent.
記載の鉄系ナノメートルスケール針状体の製造方法。11. The method for producing an iron-based nanometer-scale needle according to claim 10, wherein the reducing agent is hydrogen.
に設定する、請求項７、８、９、１０および１１に記載
の鉄系ナノメートルスケール針状体の製造方法。12. The temperature of the gas phase is 200 to 1,500 ° C.
The method for producing an iron-based nanometer-scale needle according to any one of claims 7, 8, 9, 10, and 11, wherein
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000093848A JP2001279305A (en) | 2000-03-30 | 2000-03-30 | Iron-based nanometer scale acicular body and its production method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000093848A JP2001279305A (en) | 2000-03-30 | 2000-03-30 | Iron-based nanometer scale acicular body and its production method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001279305A true JP2001279305A (en) | 2001-10-10 |
Family
ID=18608976
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000093848A Pending JP2001279305A (en) | 2000-03-30 | 2000-03-30 | Iron-based nanometer scale acicular body and its production method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001279305A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007111816A (en) * | 2005-10-19 | 2007-05-10 | National Institute For Materials Science | Multifunctional nanowire, method of manufacturing same, and concentration method using multifunctional nanowire |
| JP2013163615A (en) * | 2012-02-10 | 2013-08-22 | National Institute For Materials Science | Whisker crystal of iron-based superconductor and production method of the same |
-
2000
- 2000-03-30 JP JP2000093848A patent/JP2001279305A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007111816A (en) * | 2005-10-19 | 2007-05-10 | National Institute For Materials Science | Multifunctional nanowire, method of manufacturing same, and concentration method using multifunctional nanowire |
| JP2013163615A (en) * | 2012-02-10 | 2013-08-22 | National Institute For Materials Science | Whisker crystal of iron-based superconductor and production method of the same |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Pradhan et al. | Inclusion of crystalline iron oxide nanoparticles in uniform carbon nanotubes prepared by a template carbonization method | |
| KR100867281B1 (en) | Synthesis of Monodisperse and Highly-Crystalline Nanoparticles of Metals, Alloys, Metal Oxides, and Multi-metallic Oxides without a Size-selection Process | |
| JP4729045B2 (en) | Method for producing magnetic or metal oxide nanoparticles | |
| US7608331B2 (en) | Cladophora-form carbon comprising carbon nanomaterials radially grown on a spherical core, process for producing the same and production apparatus | |
| US20090081454A1 (en) | Carbon Nanoparticles, Production and Use Thereof | |
| Wang et al. | Synthesis of carbon encapsulated magnetic nanoparticles with giant coercivity by a spray pyrolysis approach | |
| JP5649901B2 (en) | Multi-walled carbon nanotube aggregate and method for producing the same | |
| Ibrahim et al. | Carbon coating, carburization, and high-temperature stability improvement of cobalt nanorods | |
| Teng et al. | Face-raised octahedral Co3O4 nanocrystals and their catalytic activity in the selective oxidation of alcohols | |
| Amama et al. | Dendrimer-templated Fe nanoparticles for the growth of single-wall carbon nanotubes by plasma-enhanced CVD | |
| KR20040059300A (en) | Nanostructure comprising magnetic material and nanomaterial and method for manufacturing thereof | |
| US7897131B2 (en) | Nitrogen-mediated manufacturing method of transition metal-carbon nanotube hybrid materials | |
| JP2005238142A (en) | Catalytic structure and method for producing carbon nanotube by using the same | |
| KR20150007267A (en) | Supported catalyst and carbon nanotubes preparing by using same | |
| Li et al. | Chemical synthesis and silica encapsulation of NiPt nanoparticles | |
| Csató et al. | Synthesis and characterisation of coiled carbon nanotubes | |
| US20090257944A1 (en) | Method for producing carbon nanotube | |
| Rana et al. | Preparation, texture, and magnetic properties of carbon nanotubes/nanoparticles doped with cobalt | |
| JP2001279305A (en) | Iron-based nanometer scale acicular body and its production method | |
| JP2004261630A (en) | Catalyst for manufacturing carbon nanocoil, its manufacturing method, and method for manufacturing carbon nanocoil | |
| JP2007091479A (en) | Method for production of carbon fiber | |
| Muratov et al. | Metal-carbon nanocomposites FeNi/C: production, phase composition, magnetic properties | |
| Ozkan et al. | One-step synthesis, characterization and properties of novel hybrid electromagnetic nanomaterials based on polydiphenylamine and Co–Fe particles in the absence and presence of single-walled carbon nanotubes | |
| TW200800397A (en) | Method of preparing catalyst for catalyzing carbon nanotubes growth | |
| TW200800387A (en) | Catalyst for catalyzing carbon nanotubes growth |