JPH01215718A - Titanium oxide nitride fiber and production thereof - Google Patents
Titanium oxide nitride fiber and production thereofInfo
- Publication number
- JPH01215718A JPH01215718A JP3957988A JP3957988A JPH01215718A JP H01215718 A JPH01215718 A JP H01215718A JP 3957988 A JP3957988 A JP 3957988A JP 3957988 A JP3957988 A JP 3957988A JP H01215718 A JPH01215718 A JP H01215718A
- Authority
- JP
- Japan
- Prior art keywords
- titanium oxide
- aspect ratio
- fibers
- fiber
- average length
- 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 30
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- -1 Titanium oxide nitride Chemical class 0.000 title description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 229910010303 TiOxNy Inorganic materials 0.000 claims abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 15
- 239000010936 titanium Substances 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 abstract description 10
- 239000004033 plastic Substances 0.000 abstract description 6
- 229920003023 plastic Polymers 0.000 abstract description 6
- 230000003014 reinforcing effect Effects 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 abstract description 2
- IYVLHQRADFNKAU-UHFFFAOYSA-N oxygen(2-);titanium(4+);hydrate Chemical compound O.[O-2].[O-2].[Ti+4] IYVLHQRADFNKAU-UHFFFAOYSA-N 0.000 abstract 2
- 239000000843 powder Substances 0.000 description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 7
- 229910052700 potassium Inorganic materials 0.000 description 7
- 239000011591 potassium Substances 0.000 description 7
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- KEHCHOCBAJSEKS-UHFFFAOYSA-N iron(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Fe+2] KEHCHOCBAJSEKS-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/0821—Oxynitrides of metals, boron or silicon
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は繊維状酸窒化チタンとその製造方法に関する。[Detailed description of the invention] (Industrial application field) The present invention relates to a fibrous titanium oxynitride and a method for producing the same.
このものは補強性をもった導電性の繊維であり、プラス
チック、特にエンジニアリングプラスチックやゴム、紙
、その他無機材料に添加し導電性を付与することが出来
、帯電防止材１発熱体、電波吸収体、静電記録層等に用
いられるばかりでなくプラスチックに添加した場合は機
械的性質例えば補強性、耐摩耗性１表面平滑性、加工性
、寸法安定性に優れる導電性プラスチック複合体が得ら
れる。This is a conductive fiber with reinforcing properties that can be added to plastics, especially engineering plastics, rubber, paper, and other inorganic materials to impart conductivity. In addition to being used in electrostatic recording layers and the like, when added to plastics, conductive plastic composites having excellent mechanical properties such as reinforcing properties, abrasion resistance, surface smoothness, workability, and dimensional stability can be obtained.
更に加熱反応の程度によって青色、黒色、茶色等の種々
の色を呈するため顔料としての用途も考えられる。Furthermore, since it exhibits various colors such as blue, black, and brown depending on the degree of heating reaction, it can also be used as a pigment.
（従来の技術と問題点）
導電性を示す繊維状の粉末としては、カーボン（炭素繊
維、ケッチエンブラック）、本発明者らが開発したチタ
ン酸カリウムを還元した粉末（特開昭５９−１４１４２
５）、チタン酸アルカリをカーボンで還元した粉末（特
公昭６２−３７６７）及びチタン酸カリウムにアンチモ
ンをドープした酸化スズをコーティングした粉末などが
知られている。カーボンやカーボンで還元したチタン酸
カリウムは表面が炭素質であるため、一般の無機フィラ
ーに比べて疎水性を示し、プラスチックに添加した場合
、他の顔料等となじみに＜＜、混合時の分散性、成形体
での色別れや脱離が問題となる。また本発明者らが開発
した六チタン酸カリウムを還元した粉末については８０
０℃を越える還元では元の繊維が折れやすくなる。導電
性物質をコーティングしたチタン酸カリウム繊維につい
ては導電性物質と基体との密着性が問題とされる。更に
チタン酸アルカリ繊維を母材とした導電材はポリカーボ
ネートや難燃剤を添加したエンジニアリングプラスチッ
クや半導体関連の帯電防止用途のようなアルカリの混在
をきらう用途には使用出来ないという問題がある。(Prior art and problems) Examples of fibrous powders that exhibit electrical conductivity include carbon (carbon fiber, Ketschen Black), powder obtained by reducing potassium titanate developed by the present inventors (Japanese Patent Laid-Open No. 59-14142
5), a powder obtained by reducing alkali titanate with carbon (Japanese Patent Publication No. 62-3767), and a powder obtained by coating potassium titanate with antimony-doped tin oxide are known. Carbon or potassium titanate reduced with carbon has a carbonaceous surface, so it is more hydrophobic than general inorganic fillers, and when added to plastics, it blends well with other pigments, etc., and is less likely to be dispersed during mixing. Problems arise such as color separation and detachment in molded products. In addition, regarding the powder made by reducing potassium hexatitanate developed by the present inventors, 80
When the temperature exceeds 0°C, the original fibers tend to break. Regarding potassium titanate fibers coated with a conductive substance, the adhesion between the conductive substance and the substrate is a problem. Furthermore, there is a problem in that conductive materials using alkali titanate fibers as a base material cannot be used in applications where the presence of alkali is to be avoided, such as polycarbonate, engineering plastics containing flame retardants, and antistatic applications related to semiconductors.
本発明者らは繊維状の酸化チタンもしくは水和酸化チタ
ン粉末をアンモニアを含む還元雰囲気下で加熱還元する
ことにより１元の繊維状を保持した導電性の酸窒化チタ
ン繊維が容易に得られることを見出し、先に出願した。The present inventors have discovered that electrically conductive titanium oxynitride fibers that retain their original fibrous state can be easily obtained by heating and reducing fibrous titanium oxide or hydrated titanium oxide powder in a reducing atmosphere containing ammonia. I found it and applied first.
出発原料となる水和酸化チタン繊維は、針状のチタン酸
アルカリ （−般には焼成法やフラツクス性によって得
られる四チタン酸カリウム繊維）を水または酸溶液で水
熱処理し、アルカリを除去する方法〔柳田、清水。Hydrated titanium oxide fibers, which serve as the starting material, are produced by hydrothermally treating acicular alkali titanate (generally potassium tetratitanate fibers obtained by calcination or fluxing) with water or an acid solution to remove the alkali. Method [Yanagita, Shimizu.
繊維学会誌、 ３４（１９７ｇ）、 ３１９）、板状の
チタン酸アルカリ （一般にはメルト法で得たニチタン
酸カリウム繊維）を酸水溶液で処理しアルカリを除去す
る方法〔農水、大板、窯業協会誌、９０（１９８２）、
１９〕、 または三塩化チタン水溶液を空気で酸化す
る方法〔粉体粉末冶金協会、昭和５５年度秋孕大会講演
概要集２−６、Ｐ８６） 、 によって得られること
が既に知られている。Journal of the Japan Textile Society, 34 (197g), 319), a method of removing alkali by treating plate-shaped alkali titanate (generally potassium nititanate fibers obtained by the melt method) with an aqueous acid solution [Nohsui, Ohita, Ceramics Association Magazine, 90 (1982),
19], or a method of oxidizing an aqueous titanium trichloride solution with air [Powder Metallurgy Association, 1981 Autumn Conference Abstracts 2-6, p. 86).
また酸化チタン繊維は水和酸化チタン鐵帷を数百℃以上
で加熱脱水することにより得られ、また四塩化チタンを
含有する塩化物溶融塩中で空気により酸化する方法によ
っても容易に得ることが出来る。 （Ｕ、Ｓ、Ｐ、３，
０１２，８５７．υ、Ｓ、Ｐ、３，０３０，１８３）（
問題解決に係る知見）
本発明者らは以上の既知の事項により繊維状の導電性酸
窒化チタン粉末が酸化チタン繊維もしくは水和酸化チタ
ン繊維をアンモニアを含む還元雰囲気下で加熱還元する
ことにより、効率よくえられることを見出して本発明を
完成した。Titanium oxide fibers can also be obtained by heating and dehydrating hydrated titanium oxide iron sheets at several hundred degrees Celsius or higher, and can also be easily obtained by oxidizing with air in a molten chloride salt containing titanium tetrachloride. I can do it. (U, S, P, 3,
012,857. υ, S, P, 3,030,183) (
Findings related to problem solving) Based on the above-mentioned known information, the present inventors succeeded in converting fibrous conductive titanium oxynitride powder by heating and reducing titanium oxide fibers or hydrated titanium oxide fibers in a reducing atmosphere containing ammonia. The present invention was completed after discovering that it can be obtained efficiently.
（発明の構成）
本発明は、一般式ＴｉＯｘＮｙ （１＜ ｘ ＋ ｙ
＜ ２）なる組成を有し、酸素を４〜３９ｗｔ％、窒素
を１〜２０ｖｔ％（Ｏ／Ｎ重量比３９〜０．２）含有し
た平均長０．３μ鳳〜２０００μ■（アスペクト比（長
径／短径）３〜２００）の酸窒化チタン繊維を提供する
１本発明はまた、繊維状の酸化チタンもしくは水和酸化
チタンをアンモニアを含む還元雰囲気下で５００−１０
００℃に加熱して還元することからなる導電性酸窒化チ
タン繊維の製造方法を提供する。(Structure of the Invention) The present invention has the general formula TiOxNy (1< x + y
< 2), containing 4 to 39 wt% oxygen and 1 to 20 vt% nitrogen (O/N weight ratio 39 to 0.2), average length 0.3μ to 2000μ■ (aspect ratio (longer diameter) The present invention also provides a titanium oxynitride fiber having a diameter of 500-100% (breadth diameter) of 3 to 200%.
Provided is a method for producing conductive titanium oxynitride fibers, which comprises heating to 00°C and reducing.
本発明に用いる繊維状の酸化チタンもしくは水和酸化チ
タンは無定型及びアナターゼ型、ルチル型の正方晶系の
いずれの結晶型でもよく、平均長さ０．３μｍから２０
００μｍ、アスペクト比（長径／短径）３〜２００の粉
末で、アルカリ含有量が１ｗｔ％以下のものである。平
均長さが０．３μｍ未満であると導電性複合体への添加
量が多くなる。平均長さが２０００μ重を越えると繊維
同士がからまり複合体中での分散が悪くなる。またアス
ペクト比については、３未満であると添加量が増し、補
強性などの機械的性質の向上がみられなくなる。２００
を越えると複合化の際折損し易くなり、分散性も低下す
る。カリウム、ナトリウムなどのアルカリ含有量につい
てはｌｖｔ％を越えると加熱還元時に折れ易くなるし、
本発明の繊維状の導電性酸窒化チタンがアルカリをきら
う用途に使用出来なくなる。The fibrous titanium oxide or hydrated titanium oxide used in the present invention may be of any tetragonal crystal type, such as amorphous, anatase, or rutile, and has an average length of 0.3 μm to 20 μm.
00 μm, an aspect ratio (major axis/minor axis) of 3 to 200, and an alkali content of 1 wt% or less. If the average length is less than 0.3 μm, the amount added to the conductive composite will be large. If the average length exceeds 2000μ, the fibers will become entangled with each other, resulting in poor dispersion in the composite. Regarding the aspect ratio, if it is less than 3, the amount added will increase and no improvement in mechanical properties such as reinforcing properties will be observed. 200
If it exceeds this amount, it becomes easy to break during compositing, and the dispersibility also decreases. Regarding alkali content such as potassium and sodium, if it exceeds lvt%, it will easily break during heat reduction.
The fibrous conductive titanium oxynitride of the present invention cannot be used in applications where alkalis are averse.
繊維状の酸化チタンもしくは水和酸化チタンをアンモニ
アを含む還元雰囲気下で還元する場合、元の形状を維持
し、導電性を出すためには加熱温度が重要である。この
温度範囲は５００〜１０００℃で、好ましくは、６００
〜９００℃である。５００℃未満では長時間還元雰囲気
下においても、反応が進行せず。When reducing fibrous titanium oxide or hydrated titanium oxide in a reducing atmosphere containing ammonia, the heating temperature is important in order to maintain the original shape and provide conductivity. This temperature range is 500-1000°C, preferably 600°C
~900°C. Below 500°C, the reaction does not proceed even under a reducing atmosphere for a long time.
１０００℃を越える温度では繊維同士の焼結が進み元の
形状が維持出来ず、補強性を失う、この温度範囲におい
て反応時間は０．５〜６時間の比較的短時間で良い、ア
ンモニアを含む還元性ガスの流量については、キャリー
オーバーが抑えられる範囲で炉内線速度が大きいほど均
一な粉末が得られるが少なくとも０．５ｃ■／ｓｅｅ以
上の炉内線速度がないと反応は均一に進行しない、この
ようにして得られる酸窒化チタン繊維は反応温度、時間
、還元性ガスの流量を変えることにより１０″″″Ω・
ｃｍから１０’Ω・ａｍの広範囲の導電性をもった有色
の補強性粉末が得られる。またこの繊維はＴｉ（ｌｘＮ
ｙ（１＜ ｘ ＋ｙ＜２）なる組成を有し、酸素を４〜
３９ｗｔ％、窒素を１〜２０瞥ｔ％（Ｏ７Ｎ重量比３９
〜０．２）含有する。酸素３９ｗｔ％を越え、窒素１ｗ
ｔ％未満であると導電性を示さず、また酸素４ｗｔ％未
満、窒素２０ｖｔ％を越えると元の形状が維持出来なく
なる０以上のプロセスにより得られた粉末は絶縁性材料
（プラスチックス、紙、無機物等）と複合化させること
より少ない添加量で導電性を付与することが出来る。更
に、プラスチックに添加した場合、機械的強度。If the temperature exceeds 1000℃, the fibers will sinter and cannot maintain their original shape and lose their reinforcing properties.In this temperature range, the reaction time is relatively short, 0.5 to 6 hours.Contains ammonia. Regarding the flow rate of the reducing gas, as long as carryover is suppressed, the higher the in-furnace linear velocity, the more uniform the powder can be obtained, but unless the in-furnace linear velocity is at least 0.5 c/see or higher, the reaction will not proceed uniformly. The titanium oxynitride fibers obtained in this way can be produced by changing the reaction temperature, time, and flow rate of the reducing gas.
A colored reinforcing powder is obtained with a wide range of conductivity from cm to 10' Ω·am. Also, this fiber is Ti(lxN
It has a composition of y (1< x + y<2), and contains 4~
39 wt%, 1 to 20 t% of nitrogen (O7N weight ratio 39
~0.2) Contains. Over 39wt% oxygen, 1w nitrogen
If it is less than t%, it will not show conductivity, and if it is less than 4wt% oxygen and 20vt% nitrogen, it will not be able to maintain its original shape. Conductivity can be imparted with a smaller amount of addition than by compounding with an inorganic substance (such as an inorganic substance). Furthermore, when added to plastics, mechanical strength.
寸法安定性等の向上を示す。Shows improvement in dimensional stability, etc.
以下に実施例により本発明を具体的に示す。The present invention will be specifically illustrated by examples below.
実施例１〜４
四チタン酸カリウム繊維より製造した平均繊維長さ１０
μｍ、アスペクト比３０の水和酸化チタン繊維（カリウ
ム含有量０．７ｗｔ％）２０ｇをボートに入れて。Examples 1 to 4 Average fiber length 10 produced from potassium tetratitanate fibers
20 g of hydrated titanium oxide fiber (potassium content 0.7 wt%) with an aspect ratio of 30 μm was placed in a boat.
反応温度、反応時間、反応ガスの組成と炉内線速度を変
化させて繊維状の酸窒化チタンを製造し。Fibrous titanium oxynitride was produced by varying the reaction temperature, reaction time, reaction gas composition, and furnace linear velocity.
組成、比抵抗、色、形状を測定した。結果を第１表に示
す。The composition, resistivity, color, and shape were measured. The results are shown in Table 1.
実施例５〜７
三塩化チタン水溶液より製造した平均繊維長さ０．６μ
■、アスペクト比７のルチル型酸化チタン繊維を２０ｇ
ボートに入れて反応条件を変えて処理を行った結果を第
１表に示す。Examples 5-7 Average fiber length 0.6μ produced from titanium trichloride aqueous solution
■20g of rutile-type titanium oxide fiber with an aspect ratio of 7.
Table 1 shows the results of placing the samples in a boat and performing treatments under different reaction conditions.
実施例８
板状のニチタン酸カリウム繊維から製造した平均繊維長
さ４００μｍ、アスペクト比３０のアナターゼ型酸化チ
タン繊維を２０ｇボートに入れてＮＨ，ガスを２ ｃｍ
／ｓｅｅの炉内線速度で、９００℃、ｌｈｒの処理を行
った。結果を第１表に示す。Example 8 20 g of anatase-type titanium oxide fiber with an average fiber length of 400 μm and an aspect ratio of 30 manufactured from plate-shaped potassium nititanate fibers was placed in a boat and NH and gas were added at 2 cm.
The treatment was carried out at 900° C. and lhr at an in-furnace linear velocity of /see. The results are shown in Table 1.
比較例１
実施例１と同形状のチタン酸カリウムを用い同様の反応
条件を行なって製造した。Comparative Example 1 A product was produced using potassium titanate having the same shape as in Example 1 and performing the same reaction conditions.
比較例２〜３
実施例１の反応条件を還元温度４５０℃、 １０５０
’ｃ以外は同一にし処理を行った結果を表１に示す。Comparative Examples 2 to 3 The reaction conditions of Example 1 were changed to a reduction temperature of 450°C and 1050°C.
Table 1 shows the results of the processing, with everything except 'c being the same.
実施例９
実施例３の繊維状酸窒化チタン粉末をポリプロピン（三
菱油化ＢＣ−４）に混合し、二本ロールを用い混練した
後、シート状に成形した。該シートについて表面抵抗、
引張強度を測定した結果を第２表に示す。Example 9 The fibrous titanium oxynitride powder of Example 3 was mixed with polypropyne (Mitsubishi Yuka BC-4), kneaded using two rolls, and then molded into a sheet. The surface resistance of the sheet,
The results of measuring the tensile strength are shown in Table 2.
第２表 特許出頭人三菱金属株式会社 久保田鉄工株式会社 弁理人弁理士松井政広 他１名Table 2 Patent applicant Mitsubishi Metals Corporation Kubota Iron Works Co., Ltd. Patent Attorney Masahiro Matsui and 1 other person
Claims (1)
有し、酸素を４〜３９ｗｔ％、窒素を１〜２０ｗｔ％（
Ｏ／Ｎ重量３９〜０．２）を含有した平均長０．３μｍ
〜２０００μｍ、アスペクト比（長径／短径）３〜２０
０の酸窒化チタンの繊維。 ２、繊維状の酸化チタンもしくは水和酸化チタンをアン
モニアを含む還元雰囲気下で、５００〜１０００℃にし
て加熱して還元することからなる導電性酸窒化チタン繊
維の製造法。[Claims] 1. It has the general formula TiOxNy (1<x+y<2), and contains 4 to 39 wt% of oxygen and 1 to 20 wt% of nitrogen (
Average length 0.3 μm containing O/N weight 39-0.2)
~2000μm, aspect ratio (major axis/minor axis) 3~20
0 titanium oxynitride fiber. 2. A method for producing conductive titanium oxynitride fibers, which comprises heating and reducing fibrous titanium oxide or hydrated titanium oxide at 500 to 1000° C. in a reducing atmosphere containing ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63039579A JP2612884B2 (en) | 1988-02-24 | 1988-02-24 | Titanium oxynitride fiber and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63039579A JP2612884B2 (en) | 1988-02-24 | 1988-02-24 | Titanium oxynitride fiber and its manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01215718A true JPH01215718A (en) | 1989-08-29 |
| JP2612884B2 JP2612884B2 (en) | 1997-05-21 |
Family
ID=12556994
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63039579A Expired - Lifetime JP2612884B2 (en) | 1988-02-24 | 1988-02-24 | Titanium oxynitride fiber and its manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2612884B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1138634A1 (en) * | 2000-03-31 | 2001-10-04 | Sumitomo Chemical Company, Limited | Process for producing titanium oxide |
| EP1205244A1 (en) * | 1999-08-05 | 2002-05-15 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Photocatalytic material, photocatalytic article and method for their preparation |
| JP2004335615A (en) * | 2003-05-02 | 2004-11-25 | Chiba Univ | Metal oxide semiconductor, and manufacturing method and manufacturing apparatus thereof |
| JP2009298601A (en) * | 2008-06-10 | 2009-12-24 | Sumitomo Chemical Co Ltd | Method for producing metal oxynitride |
| CZ301271B6 (en) * | 2008-05-06 | 2009-12-30 | Elmarco S.R.O. | Method for production of inorganic nanofibers and/or nanofibrous structures comprising TiN, inorganic nanofibers and/or nanofibrous structures comprising TiN and use of such nanofibrous structures |
| JP2010261098A (en) * | 2009-05-07 | 2010-11-18 | Gyoseiin Genshino Iinkai Kakuno Kenkyusho | New metal nitrogen oxide process |
-
1988
- 1988-02-24 JP JP63039579A patent/JP2612884B2/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1205244A1 (en) * | 1999-08-05 | 2002-05-15 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Photocatalytic material, photocatalytic article and method for their preparation |
| EP1205244A4 (en) * | 1999-08-05 | 2005-01-19 | Toyoda Chuo Kenkyusho Kk | Photocatalytic material, photocatalytic article and method for their preparation |
| EP1138634A1 (en) * | 2000-03-31 | 2001-10-04 | Sumitomo Chemical Company, Limited | Process for producing titanium oxide |
| US6827922B2 (en) | 2000-03-31 | 2004-12-07 | Sumitomo Chemical Company, Limited | Process for producing titanium oxide |
| JP2004335615A (en) * | 2003-05-02 | 2004-11-25 | Chiba Univ | Metal oxide semiconductor, and manufacturing method and manufacturing apparatus thereof |
| CZ301271B6 (en) * | 2008-05-06 | 2009-12-30 | Elmarco S.R.O. | Method for production of inorganic nanofibers and/or nanofibrous structures comprising TiN, inorganic nanofibers and/or nanofibrous structures comprising TiN and use of such nanofibrous structures |
| JP2009298601A (en) * | 2008-06-10 | 2009-12-24 | Sumitomo Chemical Co Ltd | Method for producing metal oxynitride |
| JP2010261098A (en) * | 2009-05-07 | 2010-11-18 | Gyoseiin Genshino Iinkai Kakuno Kenkyusho | New metal nitrogen oxide process |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2612884B2 (en) | 1997-05-21 |
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