JPS63252928A - Electrically conductive titanate fiber and production thereof - Google Patents
Electrically conductive titanate fiber and production thereofInfo
- Publication number
- JPS63252928A JPS63252928A JP8675387A JP8675387A JPS63252928A JP S63252928 A JPS63252928 A JP S63252928A JP 8675387 A JP8675387 A JP 8675387A JP 8675387 A JP8675387 A JP 8675387A JP S63252928 A JPS63252928 A JP S63252928A
- Authority
- JP
- Japan
- Prior art keywords
- fiber
- fibers
- titanate
- oxide layer
- titanium oxide
- 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.)
- Granted
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 63
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052783 alkali metal Inorganic materials 0.000 claims description 17
- -1 alkali metal titanate salt Chemical class 0.000 claims description 12
- 150000004767 nitrides Chemical group 0.000 claims 2
- 239000004033 plastic Substances 0.000 abstract description 16
- 229920003023 plastic Polymers 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract 3
- 238000010438 heat treatment Methods 0.000 description 14
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 7
- 238000005121 nitriding Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 150000001340 alkali metals Chemical class 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000011231 conductive filler Substances 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003365 glass fiber Substances 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007786 electrostatic charging Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Conductive Materials (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、導電性チタン酸塩のファイバーとその製造方
法に関し、特に導電性が要求されるプラスチック用フィ
ラーとして好適に用いられるものであって、補強効果と
表面平滑度に優れた導電性ファイバーに関連する技術に
ついて提案する。Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a conductive titanate fiber and a method for producing the same, and is particularly suitable for use as a filler for plastics that require conductivity. , we propose technology related to conductive fibers with excellent reinforcement effects and surface smoothness.
（従来の技術）
近年、電子機器類は、それ自体の急速な発展およびそれ
ら機器類ケーシングのプラスチック化に伴い、電磁波障
害や静電気帯電の問題を抱えていた。これら電磁波障害
の除去および帯電の防止についての従来技術としては、
プラスチックに各種の導電性フィラーなどを充填して該
プラスチックを導電化する技術が提案されている。例え
ば、カーボン粒子、カーボンファイバー、アルミニウム
やステンレス、真鍮などの金属粒子、あるいはそれらの
金属ファイバー、メタライズドガラスファイバー、さら
には導電性チタン酸アルカリ金属塩などの導電性フィラ
ーがそれである。(Prior Art) In recent years, electronic devices have had problems with electromagnetic interference and electrostatic charging due to their rapid development and the use of plastic for their casings. Conventional techniques for removing electromagnetic interference and preventing static electricity include:
Techniques have been proposed in which plastics are made electrically conductive by filling them with various conductive fillers. Examples include carbon particles, carbon fibers, metal particles such as aluminum, stainless steel, and brass, or metal fibers thereof, metallized glass fibers, and conductive fillers such as conductive alkali metal titanates.
上述した導電性フィラーの中でも導電性チタン酸アルカ
リ金属塩に関しての技術についても多くが提案されてお
り、例えば、特開昭５９−１０２８２０号公報、特開昭
６１−１４１６１８号公報には、チタン酸アルカリ金属
塩の表面に導電性を有する水不溶性金属化合物を沈着さ
せる技術が、また特開昭６０−２６４３２６号公報、特
開昭６１−１１７１１９号公報および特開昭６１−１９
７４２２号公報には、チタン酸塩と異種元素を含む化合
物との混合物を焼成することによりチタン酸塩に異種元
素を導入する技術が、さらに特開昭６１−５５２１７号
公報にはチタン酸カリウム繊維をアンモニアガス雰囲気
下で焼成し、酸素欠陥を形成させる技術が開示されてい
る。Among the above-mentioned conductive fillers, many techniques regarding conductive alkali metal titanates have been proposed. A technique for depositing a water-insoluble metal compound having conductivity on the surface of an alkali metal salt has also been disclosed in JP-A-60-264326, JP-A-61-117119, and JP-A-61-19.
7422 discloses a technique for introducing a different element into a titanate by firing a mixture of a titanate and a compound containing a different element, and JP-A-61-55217 discloses a technique for introducing a different element into a titanate by firing a mixture of a titanate and a compound containing a different element. A technique has been disclosed in which oxygen defects are formed by firing in an ammonia gas atmosphere.
〈発明が解決しようとする問題点）
まず、一般的な従来技術であるカーボン粒子および金属
粒子を使うものでは、プラスチックに対する補強効果が
小さいという問題点があった。次に、カーボンファイバ
ーを使うものでは、繊維径が太いためプラスチックの表
面平滑度が劣るだけでなく高価であるという問題点があ
った。また、金属ファイバーの場合も１、補強効果およ
び導電性の点では問題はないものの繊維の径が太いため
にプラスチックに充填した場合、プラスチック表面の平
滑度が劣るという問題があった。さらに、メタライズド
ガラスファイバーの場合は、ガラスファイバー表面に金
属をめっきしたものであるが、プラスチックとの混合、
成形の過程でめっきが剥がれ導電率が低下するという問
題、および繊維径が太いためプラスチックの表面平滑度
が劣るという問題とがあった。(Problems to be Solved by the Invention) First, the general prior art technology that uses carbon particles and metal particles has a problem in that the reinforcing effect on plastics is small. Next, those using carbon fiber have the problem that the fiber diameter is large, which not only results in poor surface smoothness of the plastic but also makes it expensive. In the case of metal fibers, 1. Although there is no problem in terms of reinforcing effect and conductivity, there is a problem in that the smoothness of the plastic surface is poor when the fibers are filled with plastic because the diameter of the fibers is large. Furthermore, in the case of metallized glass fiber, the glass fiber surface is plated with metal, but it is mixed with plastic,
There were problems in that the plating peeled off during the molding process and the conductivity decreased, and that the surface smoothness of the plastic was poor due to the large fiber diameter.
これに対し、上記導電性チタン酸アルカリ金属塩のファ
イバーを使うものは、繊維径が０．２〜０．５μと極め
て細いため、プラスチックの表面平滑度が高くなるだけ
でなく、補強効果も優れている。On the other hand, those using the conductive alkali metal titanate fibers have an extremely thin fiber diameter of 0.2 to 0.5μ, which not only increases the surface smoothness of the plastic but also has an excellent reinforcing effect. ing.
しかしながら、導電性の金属化合物を単に沈着させるに
すぎない従来技術の下で得られたかかるファイバーは、
チタン酸アルカリ金属塩の表面がすべて導電性物質で覆
われることはなく、また沈着させる各導電性物質自体の
導電率も低いため、導電率がｌＸｌ０−”Ω−＋ ｃ
ｍ −ｊ程度のものしか得られていない。However, such fibers obtained under prior art techniques, which merely deposit conductive metal compounds,
The surface of the alkali metal titanate salt is not entirely covered with conductive substances, and each deposited conductive substance itself has a low conductivity, so the conductivity is lXl0−”Ω−+ c
Only about m−j has been obtained.
また、チタン酸塩に異種元素を導入して導電性を付与す
る従来技術は、チタン酸塩の結晶格子中に異種元素が導
入することによりチタンイオン空格子のイオンを導いて
導電性を付与させる方法であり、１×１０°Ω−＋ ｃ
ｍ −１程度の導電率のものしか得られていなない。In addition, the conventional technology that introduces a different element into the titanate to impart electrical conductivity introduces a different element into the crystal lattice of the titanate, which guides ions in the titanium ion vacancy and imparts electrical conductivity. method, 1×10°Ω−+c
Only those with a conductivity of about m −1 have been obtained.
さらに、チタン酸カリウム繊維をアンモニアガス中で焼
成する従来技術は、焼成時間が１２０分未満と短いため
、チタン酸カリウム繊維が還元されて単に酸素欠陥が形
成されるだけに止まり、導電率が２Ｘ１０’Ω−１ｃｍ
−１程度のものしか得られていない。Furthermore, in the conventional technology in which potassium titanate fibers are fired in ammonia gas, the firing time is as short as less than 120 minutes, so the potassium titanate fibers are reduced and only oxygen defects are formed, resulting in a conductivity of 2X10. 'Ω-1cm
Only about -1 was obtained.
以上説明したように従来の導電性チタン酸アルカリ金属
塩に関する技術では、導電性の高いファイバーが得られ
ず、プラスチックに充填した時の導電性付与効果が小さ
いという大きな問題点を抱えていた。As explained above, the conventional technology relating to conductive alkali metal titanates has had the major problem that highly conductive fibers cannot be obtained and that the effect of imparting conductivity when filled into plastic is small.
本発明の目的は、上述の各種導電性フィラー。The object of the present invention is to provide the above-mentioned various conductive fillers.
特に従来の導電性チタン酸塩ファイバーの抱えている問
題点を克服できる技術を提供するところにある。In particular, it is an object of the present invention to provide a technology that can overcome the problems faced by conventional conductive titanate fibers.
（問題点を解決するための手段）
玉揚の目的に対し本発明は次の事項を要旨構成とするフ
ァイバー、すなわち、
チタン酸アルカリ金属塩からなるファイバーにおいて、
該ファイバーの酸化チタン層の少な（とも一部を窒化チ
タン化層としたことを特徴とする導電性ファイバー、
を提案する。同時に、かかるファイバーを製造する方法
として、
チタン酸アルカリ金属塩からなるファイバーを、アンモ
ニアガス雰囲気下で温度８５０〜１１００℃、時間２〜
１５時間の熱処理を施し、前記ファイバーの酸化チタン
層の一部ないし全部を窒化して窒化チタン化させること
を特徴とする導電性ファイバーの製造方法、
を提案する。(Means for Solving the Problems) For the purpose of doffing, the present invention provides a fiber comprising the following points, that is, a fiber made of an alkali metal titanate,
We propose a conductive fiber characterized in that the fiber has a small titanium oxide layer (a part of the fiber is a titanium nitride layer).At the same time, as a method for producing such a fiber, a fiber made of an alkali metal titanate salt is proposed. , under an ammonia gas atmosphere at a temperature of 850 to 1100°C for a period of 2 to
The present invention proposes a method for manufacturing a conductive fiber, which is characterized by subjecting the fiber to heat treatment for 15 hours and nitriding some or all of the titanium oxide layer of the fiber to form titanium nitride.
（作 用）
本発明において使用するチタン酸アルカリ土属塩は、一
般式Ｍ２０・ｎＴｉ０．（Ｍはアルカリ金属、ｎは１〜
１２）で示される化合物であり、チタン酸ナトリウム、
チタン酸リチウム、チタン酸カリウムなどがある。以下
に、現在工業的に生産されている四チタン酸カリウム、
六チタン酸カリウムについて説明する。(Function) The alkaline earth titanate used in the present invention has the general formula M20.nTi0. (M is an alkali metal, n is 1~
12) is a compound represented by sodium titanate,
Examples include lithium titanate and potassium titanate. Below, potassium tetratitanate currently produced industrially,
Potassium hexatitanate will be explained.
四チタン酸カリウム（Ｋ２Ｏ・４ＴｉＯ□）はＴｉｅ、
の八面体の稜および角を共有してつくる連鎖が層状構造
を形成しており、カリウムイオンがその眉間を占有する
ものである。また、六チタン酸カリウム（Ｋ！０・６Ｔ
ｉＯｚ）はＴｉｅ、八面体の連鎖がトンネル構造を形成
しており、カリウムイオンがトンネル中を占有するもの
である。これらの物質は、いずれも繊維状で合成するこ
とができるものであるが、なかでもトンネル構造を有す
る六チタン酸カリウムが最も物理的、化学的に安定で耐
熱性、機械的強度などが優れている。従って、本発明に
用いる原料として最も望ましい化合物である。Potassium tetratitanate (K2O・4TiO□) is Tie,
Chains formed by sharing the edges and corners of the octahedron form a layered structure, and potassium ions occupy the area between the eyebrows. In addition, potassium hexatitanate (K!0・6T
iOz) is a Tie, in which a chain of octahedrons forms a tunnel structure, and potassium ions occupy the inside of the tunnel. All of these substances can be synthesized in the form of fibers, but potassium hexatitanate, which has a tunnel structure, is the most physically and chemically stable, and has excellent heat resistance and mechanical strength. There is. Therefore, it is the most desirable compound as a raw material for use in the present invention.
本発明にかかるファイバーの特徴は、上述のように層状
あるいはトンネル構造を形成しているチタン酸アルカリ
金属塩について、その酸化チタン層の一部ないし全部を
、アンモニアガスにより窒化することにより、高い導電
率を有する窒化チタン層としたことにある。The fiber according to the present invention is characterized by high conductivity by nitriding part or all of the titanium oxide layer of the alkali metal titanate that forms a layered or tunnel structure as described above with ammonia gas. The reason is that the titanium nitride layer has a high ratio.
以下にチタン酸アルカリ金属塩の酸化チタン層の少な（
とも一部が、アンモニアガスによって窒化される機構に
ついて説明する。この窒化は、まず酸化チタンが高温下
でのアンモニアガス分解により生じる水素によって還元
され、次いで、この還元された低次の酸化チタンに対し
てアンモニアガスが作用し、窒化されて窒化チタンの合
成が起ると推定される。Below is a small amount of titanium oxide layer of alkali metal titanate (
The mechanism by which both parts are nitrided by ammonia gas will be explained. In this nitriding process, titanium oxide is first reduced by hydrogen produced by ammonia gas decomposition at high temperatures, and then ammonia gas acts on the reduced titanium oxide, nitriding it and synthesizing titanium nitride. It is estimated that this will occur.
このことから、熱処理の条４件は以下のように定められ
る。すなわち、雰囲気としては、アンモニアガス雰囲気
にする必要がある。熱処理の時間は、２時間未満という
短時間だと、酸化チタン層が単に還元されるだけに止ま
り、高導電率を得るのに充分な窒化チタン層が形成され
ず、一方、１５時間を越えるような長時間の熱処理は、
窒化そのものは十分に進行するものの作業効率が悪くな
り、コストが高くなると共にファイバーの強度が低下す
る。従って、本発明ファイバー製造時に採用する熱処理
時間は２時間以上１５時間以内にする必要がある。次に
、熱処理の温度は、８５０℃未満の温度では充分な窒化
が起こらず、一方、１１００℃を越えるような高温では
ファイバーの強度が低下する。From this, the four conditions for heat treatment are determined as follows. That is, the atmosphere needs to be an ammonia gas atmosphere. If the heat treatment time is short, less than 2 hours, the titanium oxide layer will simply be reduced, and a titanium nitride layer sufficient to obtain high conductivity will not be formed. The long-term heat treatment is
Although nitriding itself progresses satisfactorily, the working efficiency deteriorates, the cost increases, and the strength of the fiber decreases. Therefore, the heat treatment time employed during production of the fiber of the present invention must be from 2 hours to 15 hours. Next, if the heat treatment temperature is lower than 850°C, sufficient nitriding will not occur, while if the temperature is higher than 1100°C, the strength of the fiber will decrease.
従って、該熱処理の温度は８５０℃以上１１００℃以下
にする必要がある。Therefore, the temperature of the heat treatment needs to be 850°C or more and 1100°C or less.
以上説明したような条件にて熱処理をすると、原料であ
るチタン酸アルカリ金属塩に対する生成窒化チタンの割
合（以下「窒化チタン化率」という）が１８％以上とな
る。When the heat treatment is performed under the conditions described above, the ratio of the produced titanium nitride to the raw material alkali metal titanate (hereinafter referred to as "titanium nitride ratio") becomes 18% or more.
なお、窒化チタンの導電機構は高い導電率を示す金属伝
導であり、本発明の導電性チ、タン酸塩ファイバーは、
チタン酸アルカリ金属塩の大部分を形成している酸化チ
タン層の一部ないし全部を、かかる窒化チタンにしたも
のであり、従来の導電性チタン酸アルカリ金属塩には見
られない１×１０２Ω−＋ ｃ ｍ −ｒ以上という高
い導電率を示すものである。The electrical conductivity mechanism of titanium nitride is metallic conduction that exhibits high electrical conductivity, and the electrically conductive titanium/tanate fiber of the present invention
Part or all of the titanium oxide layer that forms most of the alkali metal titanate is made of such titanium nitride, and it has a resistance of 1 x 102 Ω-, which is not found in conventional conductive alkali metal titanates. It exhibits a high electrical conductivity of + cm -r or more.
（実施例）
チタン酸アルカリ金属塩からなるファイバーである市販
のチタン酸カリウムファイバー〔繊維径０．２〜０．５
μ、繊維長１０〜２０μ、大尽化学（株）、商品名ティ
スモＤ）５ｇを、アルミナ製ボードに載せ、これを内径
３０１ｍのアルミナ管内に挿入する。(Example) Commercially available potassium titanate fiber, which is a fiber made of alkali metal titanate [fiber diameter 0.2 to 0.5
μ, fiber length 10 to 20 μ, manufactured by Daijin Kagaku Co., Ltd., trade name Tismo D) 5 g was placed on an alumina board, and this was inserted into an alumina tube having an inner diameter of 301 m.
次に、前記アルミナ管内の空気を窒素ガスを導入してこ
れと置換し、その後アンモニアガスを０．３ｄ／■ｉｎ
、の流量にて流入しながら該管を電気炉内に設置して加
熱する。この加熱はチタン酸カリウム挿入部の管内温度
を１０℃／ｗｉｎ、の速度にて９００℃まで昇温させる
内容で行った。そして、前記温度にて２時間保持した後
、アンモニアガスの流入を止め、窒素ガスを１．０Ｍ１
７ｗ１ｎ、の流量にて流しながら常温まで冷却し、本発
明の導電性ファイバーを得た。Next, nitrogen gas is introduced to replace the air in the alumina tube, and then ammonia gas is introduced at a rate of 0.3 d/inch.
The tube is placed in an electric furnace and heated while flowing at a flow rate of . This heating was carried out to raise the temperature inside the tube of the potassium titanate insertion portion to 900° C. at a rate of 10° C./win. After maintaining the above temperature for 2 hours, the inflow of ammonia gas was stopped and nitrogen gas was added at 1.0M1.
The conductive fiber of the present invention was obtained by cooling to room temperature while flowing at a flow rate of 7w1n.
このようにして得られた導電性ファイバーについてＸ線
分析することにより、窒化チタンが形成されていること
を確認し、以下に述べる方法により導電率および窒化率
を測定した。その測定の結果を熱処理条件とともに第１
表にまとめて示す。The formation of titanium nitride was confirmed by X-ray analysis of the conductive fiber thus obtained, and the conductivity and nitridation rate were measured by the methods described below. The results of the measurement are summarized in the first step along with the heat treatment conditions.
They are summarized in the table.
ｍぼりわＬが汰
導電率の測定に当っては、まず試料０．８ｇを内径１０
鰭の金型にて１０ｋｇ／ｃ＋＊”の圧力で１０分間加圧
成型した円柱状の試験片を作成し、この試験片の厚さと
断面積を測定した後に両面に金を蒸着し、これを電極と
してその両極に常温、大気中にて直流定電圧を印加し、
その時に流れる電流値を測定した。When measuring conductivity, first measure 0.8 g of sample with an inner diameter of 10 mm.
A cylindrical test piece was created by pressure molding in a fin mold for 10 minutes at a pressure of 10 kg/c + A constant DC voltage is applied to both electrodes at room temperature and in the atmosphere.
The value of the current flowing at that time was measured.
そして、導電率は次式により算出した。Then, the conductivity was calculated using the following formula.
窒化率は、チタン酸カリウムファイバーの熱処理前と熱
処理後の重量を測定し、次式から算出した。The nitriding rate was calculated from the following formula by measuring the weight of the potassium titanate fiber before and after the heat treatment.
Ａ：熱処理前のチタン酸カリウムファイバーの重量
Ｂ：熱処理後のファイバーの重量
（発明の効果）
以上の説明ならびに実施例の結果から判るように、本発
明にかかる導電性チタン酸塩のファイバーは、ファイバ
ーの酸化チタン層の一部ないし全部を金属伝導を示す窒
化チタンに変化させたものであるから、高い導電率を示
す。しかも、繊維の径も細いのでプラスチック補強材と
して用いたときのプラスチック表面平滑度が優れるとい
う特徴を有する。A: Weight of potassium titanate fiber before heat treatment B: Weight of fiber after heat treatment (effect of the invention) As can be seen from the above explanation and the results of the examples, the conductive titanate fiber according to the present invention has the following properties: Since part or all of the titanium oxide layer of the fiber is changed to titanium nitride, which exhibits metal conductivity, it exhibits high electrical conductivity. Moreover, since the diameter of the fibers is small, the plastic surface smoothness is excellent when used as a plastic reinforcing material.
また、本発明製造方法は、熱処理時間および熱処理温度
を変えることにより、ファイバーの窒化率の制御が可能
であり、その結果、種々の導電率を示す各種の導電性フ
ァイバーを製造することができる。Furthermore, the manufacturing method of the present invention allows the nitridation rate of the fiber to be controlled by changing the heat treatment time and temperature, and as a result, various conductive fibers exhibiting various conductivities can be manufactured.
以上の説明から判るように、本発明の導電性チタン酸塩
ファイバーは、電磁波シールド、帯電防止などを目的と
した導電性プラスチックのフィラーとして好適である。As can be seen from the above description, the conductive titanate fiber of the present invention is suitable as a filler for conductive plastics for purposes such as electromagnetic shielding and antistatic properties.
Claims (1)
て、該ファイバーの酸化チタン層の少なくとも一部を窒
化チタン化層としたことを特徴とする導電性チタン酸塩
のファイバー。 ２、上記ファイバーの導電率が１×１０＾２Ω＾−＾１
ｃｍ＾−＾１以上であることを特徴とする特許請求の範
囲第１項記載のファイバー。 ３、酸化チタン層の窒化チタン化率が１８％以上である
ことを特徴とする特許請求の範囲第１項および第２項記
載の導電性ファイバー。 ４、チタン酸アルカリ金属塩からなるファイバーを、ア
ンモニアガス雰囲気下で、温度８５０〜１１００℃、時
間２〜１５時間の熱処理を施し、前記ファイバーの酸化
チタン層の一部ないし全部を窒化して窒化チタン化させ
ることを特徴とする導電性ファイバーの製造方法。[Scope of Claims] 1. A conductive titanate fiber made of an alkali metal titanate salt, characterized in that at least a part of the titanium oxide layer of the fiber is a nitride titanation layer. 2. The conductivity of the above fiber is 1×10^2Ω^-^1
The fiber according to claim 1, characterized in that the fiber has a diameter of cm^-^1 or more. 3. The conductive fiber according to claims 1 and 2, wherein the titanium nitride ratio of the titanium oxide layer is 18% or more. 4. A fiber made of an alkali metal titanate salt is heat-treated in an ammonia gas atmosphere at a temperature of 850 to 1100°C for 2 to 15 hours to nitride part or all of the titanium oxide layer of the fiber. A method for producing a conductive fiber characterized by titanizing it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8675387A JPS63252928A (en) | 1987-04-10 | 1987-04-10 | Electrically conductive titanate fiber and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8675387A JPS63252928A (en) | 1987-04-10 | 1987-04-10 | Electrically conductive titanate fiber and production thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63252928A true JPS63252928A (en) | 1988-10-20 |
| JPH0527573B2 JPH0527573B2 (en) | 1993-04-21 |
Family
ID=13895522
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8675387A Granted JPS63252928A (en) | 1987-04-10 | 1987-04-10 | Electrically conductive titanate fiber and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63252928A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0397974A (en) * | 1989-09-08 | 1991-04-23 | Ibiden Co Ltd | Electroconductive ceramic fiber and production thereof |
| US5118488A (en) * | 1990-08-28 | 1992-06-02 | Martin Marietta Energy Systems, Inc. | Process for making whiskers, fibers and flakes of transition metal compounds |
| JP2011190162A (en) * | 2010-02-17 | 2011-09-29 | Ishihara Sangyo Kaisha Ltd | Electroconductive oxide particle, treatment method of oxide particle for obtaining the same, electrode active material containing the electroconductive oxide particle, and power storage device using the electrode active material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60260425A (en) * | 1984-06-02 | 1985-12-23 | Otsuka Chem Co Ltd | Manufacture of reduced alkali metallic titanate |
-
1987
- 1987-04-10 JP JP8675387A patent/JPS63252928A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60260425A (en) * | 1984-06-02 | 1985-12-23 | Otsuka Chem Co Ltd | Manufacture of reduced alkali metallic titanate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0397974A (en) * | 1989-09-08 | 1991-04-23 | Ibiden Co Ltd | Electroconductive ceramic fiber and production thereof |
| US5118488A (en) * | 1990-08-28 | 1992-06-02 | Martin Marietta Energy Systems, Inc. | Process for making whiskers, fibers and flakes of transition metal compounds |
| JP2011190162A (en) * | 2010-02-17 | 2011-09-29 | Ishihara Sangyo Kaisha Ltd | Electroconductive oxide particle, treatment method of oxide particle for obtaining the same, electrode active material containing the electroconductive oxide particle, and power storage device using the electrode active material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0527573B2 (en) | 1993-04-21 |
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