JPH03208897A - Production of tic whisker - Google Patents
Production of tic whiskerInfo
- Publication number
- JPH03208897A JPH03208897A JP311090A JP311090A JPH03208897A JP H03208897 A JPH03208897 A JP H03208897A JP 311090 A JP311090 A JP 311090A JP 311090 A JP311090 A JP 311090A JP H03208897 A JPH03208897 A JP H03208897A
- Authority
- JP
- Japan
- Prior art keywords
- whiskers
- tic
- reaction
- hydrogen
- titanium tetrachloride
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 19
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 6
- 150000003624 transition metals Chemical class 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 11
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000010574 gas phase reaction Methods 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 15
- 239000010936 titanium Substances 0.000 abstract description 15
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052719 titanium Inorganic materials 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000008246 gaseous mixture Substances 0.000 abstract 3
- 239000004215 Carbon black (E152) Substances 0.000 abstract 2
- 229910003074 TiCl4 Inorganic materials 0.000 abstract 2
- 229930195733 hydrocarbon Natural products 0.000 abstract 2
- 150000002430 hydrocarbons Chemical class 0.000 abstract 2
- 239000012808 vapor phase Substances 0.000 abstract 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000002994 raw material Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 229910052759 nickel Inorganic materials 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- -1 Au as a catalyst Chemical class 0.000 description 2
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011151 fibre-reinforced plastic Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012779 reinforcing material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、繊維強化プラスチック（ＦＲＰ）や繊維強化
金属（ＦＲＭ）、繊維強化セラミックス（ＦＲＣ）等の
複合材料の強化材として有用な高純度で高品質なＴｉＣ
ウィスカーの製造法に関するものである。[Detailed Description of the Invention] [Field of Industrial Application] The present invention provides a highly pure reinforcing material useful as a reinforcing material for composite materials such as fiber-reinforced plastics (FRP), fiber-reinforced metals (FRM), and fiber-reinforced ceramics (FRC). high quality TiC
This invention relates to a method for producing whiskers.
［従来技術］
ＴｉＣウィスカーの製造法としては、従来より気相法に
よる方法が知られており、例えば、四塩化チタン−メタ
ン−水素系から触媒にニッケル等の金属あるいはムライ
ト等の耐火酸化物を用いて、１０５０〜１４５０℃でＴ
ｉＣウィスカーを製造する方法［Ｊｏｒｎａｌ ｏｆ
Ｃｒｙｓｔａｌ Ｇｒｏｗｔｈ ４ｆｉ（１９７９）２
２１〜２３７］や触媒となるＡｕ等の貴金属塩の水溶液
を含浸、乾燥させた黒鉛および活性炭からなる成形体上
に、ハロゲン化チタンーー酸化炭素−水素系からＴｉＣ
ウィスカーを１１００〜１４００℃で合成する方法（特
公昭５９−４５６３８号）、あるいは四塩化チタン−プ
ロパン−水素系からマンガン等の金属触媒を用いて１２
４０〜１２８０℃でＴｉＣウィスカーを合成する方法（
Ｊ、Ｅｌｅｃｔｒｏｃｈｅ＋＋＋、Ｓｏｃ、Ｌ１２（１
９７０）５４１〜５４５）が知られている。四塩化チタ
ン−メタン−水素系の方法においてはカーボン源として
高価なメタンを用いるためコスト高となり、またハロゲ
ン化チタンーー酸化炭素−水素系の方法においては、カ
ーボン源に一酸化炭素を用いるため合成されるＴｉＣウ
ィスカー中に酸素が混入し、高純度で高品質なＴｉＣウ
ィスカーが得られない。また、触媒となる貴金属塩は一
般に高価である。さらに四塩化チタン−プロパン−水素
系からマンガン等の金属触媒を用いる方法においてはウ
ィスカーの収率が十分には高くない。[Prior Art] As a method for producing TiC whiskers, a gas phase method has been known for a long time. T at 1050-1450℃ using
Method of manufacturing iC whiskers [Journal of
Crystal Growth 4fi (1979) 2
21-237] and an aqueous solution of a noble metal salt such as Au as a catalyst, and dried graphite and activated carbon.
A method of synthesizing whiskers at 1,100 to 1,400°C (Japanese Patent Publication No. 59-45638), or a method of synthesizing whiskers from a titanium tetrachloride-propane-hydrogen system using a metal catalyst such as manganese.
Method for synthesizing TiC whiskers at 40-1280°C (
J, Electroche+++, Soc, L12 (1
970) 541-545) are known. The titanium tetrachloride-methane-hydrogen system uses expensive methane as the carbon source, resulting in high costs, while the titanium halide-carbon oxide-hydrogen system uses carbon monoxide as the carbon source, making it difficult to synthesize. Oxygen gets mixed into the TiC whiskers, making it impossible to obtain high purity and high quality TiC whiskers. Furthermore, noble metal salts serving as catalysts are generally expensive. Furthermore, in the method using a metal catalyst such as manganese from a titanium tetrachloride-propane-hydrogen system, the yield of whiskers is not sufficiently high.
〔問題点を解決するための手段］
本発明者らはかかる従来の方法における問題点に鑑み、
鋭意検討の結果、カーボン源として芳香族炭化水素化合
物を用いた場合には、高純度で高品質なＴｉＣウィスカ
ーを効率よく製造できることを見出し本発明に到達した
。すなわち本発明は、遷移金属またはその化合物を含む
系内にて、四塩化チタン、芳香族炭化水素および水素か
らなる混合ガスを、反応温度１１００〜１３５０℃で気
相反応させることを特徴とするＴｉＣウィスカーの製造
法である。[Means for solving the problems] In view of the problems in the conventional methods, the present inventors
As a result of extensive studies, we have discovered that when aromatic hydrocarbon compounds are used as carbon sources, it is possible to efficiently produce TiC whiskers with high purity and high quality, and we have arrived at the present invention. That is, the present invention provides TiC, which is characterized in that a mixed gas consisting of titanium tetrachloride, an aromatic hydrocarbon, and hydrogen is subjected to a gas phase reaction at a reaction temperature of 1100 to 1350°C in a system containing a transition metal or a compound thereof. This is a method for producing whiskers.
本発明において触媒として用いる遷移金属は、ニッケル
、コバルト、鉄等が好ましい。また炭素源として用いる
芳香族炭化水素としては、ベンゼン、トルエン、キシレ
ン等が好ましく、蒸気圧が高く、反応器への供給が容易
なベンゼンが特に好ましい。また反応温度は１１００〜
１３５０℃の範囲が好ましい。この範囲を越えると生成
物は粉末が主となり、この範囲より低いと膜の生成が主
となり、いずれもＴｉＣウィスカーの収率が低くなる。The transition metal used as a catalyst in the present invention is preferably nickel, cobalt, iron, or the like. Further, as the aromatic hydrocarbon used as a carbon source, benzene, toluene, xylene, etc. are preferable, and benzene is particularly preferable because it has a high vapor pressure and can be easily supplied to the reactor. Also, the reaction temperature is 1100~
A range of 1350°C is preferred. Above this range, the product will be mainly powder, and below this range, the product will mainly be a film, and in both cases the yield of TiC whiskers will be low.
原料ガス中の四塩化チタンと芳香族炭化水素の混合比率
はカーボンとチタンの原子比で０．８〜３．０の範囲が
好ましい。Ｃ／Ｔｉ＜０．８の場合、生成物は膜が主と
なる。またＣ／Ｔｉ＞３の場合には形状のイビツな針状
結晶や粉末が得られる易くなる。The mixing ratio of titanium tetrachloride and aromatic hydrocarbon in the raw material gas is preferably in the range of 0.8 to 3.0 in terms of the atomic ratio of carbon to titanium. When C/Ti<0.8, the product is mainly a film. Further, when C/Ti>3, it becomes easier to obtain irregularly shaped needle-like crystals or powder.
以下実施例により本発明を具体的に説明する。The present invention will be specifically explained below using Examples.
実施例１
内径３５ｍｍ、長さ１０００ｍ ｍのアルミナ管からな
る反応管を具備した横型流通方式の熱ＣＶｂ装置を用い
て反応をおこなった。以下の実施例、比較例のいずれも
同じ装置を用いておこなった。Example 1 A reaction was carried out using a horizontal flow type thermal CVb apparatus equipped with a reaction tube made of an alumina tube with an inner diameter of 35 mm and a length of 1000 mm. The following examples and comparative examples were all carried out using the same apparatus.
反応管の中央に幅２０ｍ ｍ 、長さ２００ｍｍ、厚さ
３ｍｍのニッケル板を設置し、反応管中央を１２００℃
に加熱、保持した。その後四塩化チタン、ベンゼンおよ
び水素からなる原料ガスを以下に示す流量にて導入した
。なお、反応圧力は大気圧である。A nickel plate with a width of 20 mm, a length of 200 mm, and a thickness of 3 mm was installed in the center of the reaction tube, and the center of the reaction tube was heated to 1200°C.
heated and held. Thereafter, a raw material gas consisting of titanium tetrachloride, benzene, and hydrogen was introduced at the flow rate shown below. Note that the reaction pressure is atmospheric pressure.
四塩化チタｙ：５１ｓｃｃｍ
ベンゼン ：１５ｓｅｃｍ
水素 ：２，５ｇ１ｍ
Ｃ／Ｔｉ ：１．８
６０分間反応後ニッケル板を取り出すと、板の上に約２
．６ｇのウィスカーが生成していた。このウィスカーを
ＳＥＭ観察したところ、直径１０μｍ以下の形状良好な
ウィスカーであった。また、Ｘ線回折パターンはＴｉＣ
のそれと良好に一致した。Titanium tetrachloride: 51 sccm Benzene: 15 sec Hydrogen: 2.5 g 1 m C/Ti: 1.8 When the nickel plate is taken out after 60 minutes of reaction, about 2
．． 6g of whiskers were produced. When this whisker was observed by SEM, it was found to be a whisker with a diameter of 10 μm or less and a good shape. In addition, the X-ray diffraction pattern is TiC
It was in good agreement with that of .
第１図はＴｉＣウィスカーの繊維形状を示すＳＥＭ写真
である。FIG. 1 is a SEM photograph showing the fiber shape of TiC whiskers.
実施例２
反応管の中央に幅２０ｍ ｍ 、長さ２００ｍｍ、厚さ
３ｍｍのニッケル板を設置し、反応管中央を１１５０℃
に加熱、保持した。その後、四塩化チタン、ベンゼンお
よび水素からなる原料ガスを以下に示す流量にて導入し
た。なお、反応圧力は大気圧である。Example 2 A nickel plate with a width of 20 mm, a length of 200 mm, and a thickness of 3 mm was installed in the center of a reaction tube, and the center of the reaction tube was heated to 1150°C.
heated and held. Thereafter, a raw material gas consisting of titanium tetrachloride, benzene, and hydrogen was introduced at the flow rate shown below. Note that the reaction pressure is atmospheric pressure.
四塩化チタン：５４ｓｃｃｍ
ベンゼン ＝２５ＳＣＣｍ
水素 ：３．５ｇ１ｍ
Ｃ／Ｔｉ ：２．３
６０分間反応後ニッケル板を取り出すと、板の上に約２
．０ｇのウィスカーが生成していた。このウィスカーを
ＳＥＭ観察したところ、直径１０μｍ以下の形状良好な
ウィスカーであった。またＸ線回折パターンはＴｉＣの
それとよく一致した。Titanium tetrachloride: 54sccm Benzene = 25SCCm Hydrogen: 3.5g1m C/Ti: 2.3 When the nickel plate was taken out after 60 minutes of reaction, about 2
．． 0g whiskers were generated. When this whisker was observed by SEM, it was found to be a whisker with a diameter of 10 μm or less and a good shape. Moreover, the X-ray diffraction pattern matched well with that of TiC.
実施例３
１モル／Ｉ！の塩化ニッケル水溶液を含浸、乾燥した黒
鉛板（幅２０ｍｍ、長さ２００ｍｍ、厚さ５ ｍ ｍ
）を反応管の中央に設置し、反応管中央を１２５０℃に
加熱、保持した。その後、四塩化チタン、ベンゼンおよ
び水素からなる原料ガスを以下に示す流量にて導入した
。なお、反応圧力は大気圧である。Example 3 1 mol/I! A graphite plate (width 20 mm, length 200 mm, thickness 5 mm) impregnated with nickel chloride aqueous solution and dried
) was placed in the center of the reaction tube, and the center of the reaction tube was heated and maintained at 1250°C. Thereafter, a raw material gas consisting of titanium tetrachloride, benzene, and hydrogen was introduced at the flow rates shown below. Note that the reaction pressure is atmospheric pressure.
四塩化チタ７：６１ｓｃｃｍ
ベンゼン ：９ｓｅｃｍ
水素 ：２．Ｏ５１ｍ
Ｃ／Ｔｉ ：０．８９
３０分間反応後黒鉛板を取り出すと、板の上に約０．９
ｇのウィスカーが生成していた。このウィスカーをＳＥ
Ｍ観察したところ、直径１０ｍｍ以下の形状良好なウィ
スカーであった。また、Ｘ線回折パターンはＴｉＣのそ
れと良好に一致した。Titanium tetrachloride 7: 61sccm Benzene: 9secm Hydrogen: 2. O51m C/Ti: 0.89 When the graphite plate is taken out after 30 minutes of reaction, about 0.9
g whiskers were generated. SE this whisker
M observation revealed that the whiskers had a diameter of 10 mm or less and had a good shape. Moreover, the X-ray diffraction pattern matched well with that of TiC.
実施例４
０．２モル／１の塩化ニッケル水溶液を含浸、乾燥した
黒鉛板（幅２０ｍｍ、長さ２００ｍｍ、厚さ５ｍｍ）を
反応管の中央に設置し、反応管中央を１２５０℃に加熱
、保持した。その後、四塩化チタン、ベンゼンおよび水
素からなる原料ガスを以下に示す流量にて導入した。な
お、反応圧力は大気圧である。Example 4 A graphite plate (width 20 mm, length 200 mm, thickness 5 mm) impregnated with a 0.2 mol/1 nickel chloride aqueous solution and dried was placed in the center of a reaction tube, and the center of the reaction tube was heated to 1250°C. held. Thereafter, a raw material gas consisting of titanium tetrachloride, benzene, and hydrogen was introduced at the flow rates shown below. Note that the reaction pressure is atmospheric pressure.
四塩化チタン：５１ｓｃｃｍ
ベンゼン ：１２ｓｅｃｍ
水素 ：１，５ｇ１ｍ
Ｃ／Ｔｉ ：１．２
３０分間反応後黒鉛板を取り出すと、板の上に約１．７
ｇのウィスカーが生成していた。このウィスカーをＳＥ
Ｍ観察したところ、直径１０ｍｍ以下の形状良好なウィ
スカーであった。また、Ｘ線回折パターンはＴｉＣのそ
れと良好に一致した。Titanium tetrachloride: 51sccm Benzene: 12secm Hydrogen: 1.5g1m C/Ti: 1.2 When the graphite plate is taken out after 30 minutes of reaction, about 1.7
g whiskers were generated. SE this whisker
M observation revealed that the whiskers had a diameter of 10 mm or less and had a good shape. Moreover, the X-ray diffraction pattern matched well with that of TiC.
実施例５
１モル／ｌの硝酸コバルト水溶液を含浸、乾燥した黒鉛
板（輻２０ｍｍ、長さ２００ｍｍ、厚さ５ｍｍ）を反応
管の中央に設置し、反応管中央を１２５０℃に加熱、保
持した。その後、四塩化チタン、ベンゼンおよび水素か
らなる原料ガスを以下に示す流量にて導入した。なお、
反応圧力は大気圧である。Example 5 A dried graphite plate (radius 20 mm, length 200 mm, thickness 5 mm) impregnated with 1 mol/l aqueous cobalt nitrate solution was placed in the center of a reaction tube, and the center of the reaction tube was heated and maintained at 1250°C. . Thereafter, a raw material gas consisting of titanium tetrachloride, benzene, and hydrogen was introduced at the flow rate shown below. In addition,
The reaction pressure is atmospheric pressure.
四塩化チタン：６５ｓｃｃｍ
ベンゼン ：２Ｑｓｅｃｍ
水素 ：１，５ｇ１ｍ
Ｃ／Ｔｉ ：１．８
６０分間反応後黒鉛板を取り出すと、板の上に約１．１
ｇのウィスカーが生成していた。このウィスカーをＳＥ
Ｍ観察したところ、直径１０ｍｍ以下の形状良好なウィ
スカーであった。また、Ｘ線回折パターンはＴｉＣのそ
れと良好に一致した。Titanium tetrachloride: 65sccm Benzene: 2Qsecm Hydrogen: 1.5g1m C/Ti: 1.8 When the graphite plate is taken out after 60 minutes of reaction, approximately 1.1
g whiskers were generated. SE this whisker
M observation revealed that the whiskers had a diameter of 10 mm or less and had a good shape. Moreover, the X-ray diffraction pattern matched well with that of TiC.
実施例６
反応管の中央に幅２０ｍｍ、長さ２００ｍｍ、厚さ３ｍ
ｍの鉄板を設置し、反応管中央を１３ｐＯ℃に加熱、保
持した。その後、四塩化チタン、ベンゼンおよび水素か
らなる原料ガスを以下に示す流量にて導入した。なお、
反応圧力は大気圧である。Example 6 In the center of the reaction tube, the width is 20 mm, the length is 200 mm, and the thickness is 3 m.
An iron plate of 200 m was installed, and the center of the reaction tube was heated and maintained at 13 pO°C. Thereafter, a raw material gas consisting of titanium tetrachloride, benzene, and hydrogen was introduced at the flow rates shown below. In addition,
The reaction pressure is atmospheric pressure.
四塩化チタン：５７ｓｅｃｍ
ベンゼン ：１９ｓｅｃｍ
水素 ：１．５ｇ１ｍ
Ｃ／Ｔｉ ：１．７
６０分間反応後鉄板を取り出すと、板の上に約１゜５ｇ
のウィスカーが生成していた。このウィスカーをＳＥＭ
観察したところ、直径１０μｍ以下の形状良好なウィス
カーであった。またＸ線回折パターンはＴｉＣのそれと
よく一致した。Titanium tetrachloride: 57 sec Benzene: 19 sec Hydrogen: 1.5 g 1 m C/Ti: 1.7 When the iron plate is taken out after 60 minutes of reaction, about 1°5 g is on the plate.
whiskers were generated. SEM of this whisker
Upon observation, it was found that the whiskers had a diameter of 10 μm or less and had a good shape. Moreover, the X-ray diffraction pattern matched well with that of TiC.
実施例７
反応管の中央に幅２０ｍｍ、長さ２００ｍｍ、厚さ３ｍ
ｍのニッケル板を設置し、反応管中央を１１５０℃に加
熱、保持した。その後、四塩化チタン、トルエンおよび
水素からなる原料ガスを以下に示す流量にて導入した。Example 7 In the center of the reaction tube, the width is 20 mm, the length is 200 mm, and the thickness is 3 m.
A nickel plate of 500 m was installed, and the center of the reaction tube was heated and maintained at 1150°C. Thereafter, a raw material gas consisting of titanium tetrachloride, toluene, and hydrogen was introduced at the flow rates shown below.
なお、反応圧力は大気圧である。Note that the reaction pressure is atmospheric pressure.
四塩化チタン：５４ｓｃｃｍ
トルエン ：２５ｓｅｃｍ
水素 ：３．５ｇ１ｍ
Ｃ／Ｔｉ ：２．７
６０分間反応後ニッケル板を取り出すと、板の上に約１
．９ｇのウィスカーが生成していた。このウィスカーを
ＳＥＭ観察したところ、直径１０μｍ以下の形状良好な
ウィスカーであった。またＸ線回折パターンはＴｉＣの
それとよ（一致した。Titanium tetrachloride: 54sccm Toluene: 25secm Hydrogen: 3.5g1m C/Ti: 2.7 When the nickel plate is taken out after 60 minutes of reaction, about 1
．． 9g of whiskers were produced. When this whisker was observed by SEM, it was found to be a whisker with a diameter of 10 μm or less and a good shape. The X-ray diffraction pattern also matched that of TiC.
［発明の効果］
本発明の方法によれば、安価に酸素の混入のない高純度
で高品質なＴｉＣウィスカーを収率よく製造することが
できるものである。[Effects of the Invention] According to the method of the present invention, high purity and high quality TiC whiskers free from oxygen contamination can be produced at low cost and with good yield.
第１図は実施例１で得たＴｉＣウィスカーの繊維形状を
示すＳＥＭ写真である。
第
１
図
ｏｓｍFIG. 1 is a SEM photograph showing the fiber shape of the TiC whiskers obtained in Example 1. Figure 1 osm
Claims (1)
ン、芳香族炭化水素および水素からなる混合ガスを、反
応温度１１００〜１３５０℃で気相反応させることを特
徴とするＴｉＣウィスカーの製造法。A method for producing TiC whiskers, which comprises causing a gas phase reaction of a mixed gas consisting of titanium tetrachloride, an aromatic hydrocarbon, and hydrogen at a reaction temperature of 1100 to 1350°C in a system containing a transition metal or a compound thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP311090A JPH03208897A (en) | 1990-01-10 | 1990-01-10 | Production of tic whisker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP311090A JPH03208897A (en) | 1990-01-10 | 1990-01-10 | Production of tic whisker |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03208897A true JPH03208897A (en) | 1991-09-12 |
| JPH0583518B2 JPH0583518B2 (en) | 1993-11-26 |
Family
ID=11548213
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP311090A Granted JPH03208897A (en) | 1990-01-10 | 1990-01-10 | Production of tic whisker |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03208897A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5336291A (en) * | 1992-07-02 | 1994-08-09 | Toyota Jidosha Kabushiki Kaisha | Method of production of a metallic composite material incorporating metal carbide particles dispersed therein |
| US5441697A (en) * | 1992-08-06 | 1995-08-15 | Toyota Jidosha Kabushiki Kaisha | Method of producing TiC whiskers and metallic composites reinforced by TiC whiskers |
-
1990
- 1990-01-10 JP JP311090A patent/JPH03208897A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5336291A (en) * | 1992-07-02 | 1994-08-09 | Toyota Jidosha Kabushiki Kaisha | Method of production of a metallic composite material incorporating metal carbide particles dispersed therein |
| US5441697A (en) * | 1992-08-06 | 1995-08-15 | Toyota Jidosha Kabushiki Kaisha | Method of producing TiC whiskers and metallic composites reinforced by TiC whiskers |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0583518B2 (en) | 1993-11-26 |
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