JPS5976802A - Manufacture of hyperfine powder of titanium nitride by vapor phase reaction - Google Patents
Manufacture of hyperfine powder of titanium nitride by vapor phase reactionInfo
- Publication number
- JPS5976802A JPS5976802A JP18678982A JP18678982A JPS5976802A JP S5976802 A JPS5976802 A JP S5976802A JP 18678982 A JP18678982 A JP 18678982A JP 18678982 A JP18678982 A JP 18678982A JP S5976802 A JPS5976802 A JP S5976802A
- Authority
- JP
- Japan
- Prior art keywords
- titanium nitride
- reaction
- ammonia
- manufacture
- powder
- 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
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 25
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000012808 vapor phase Substances 0.000 title 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 13
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 15
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 8
- 239000010936 titanium Substances 0.000 abstract description 8
- 239000007795 chemical reaction product Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910010421 TiNx Inorganic materials 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- -1 titanium hydride Chemical compound 0.000 description 4
- 238000010574 gas phase reaction Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000048 titanium hydride Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 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
- 239000012300 argon atmosphere Substances 0.000 description 1
- ZHTOIEDMLUUKDZ-UHFFFAOYSA-J azane titanium(4+) tetrachloride Chemical class N.[Cl-].[Cl-].[Cl-].[Cl-].[Ti+4] ZHTOIEDMLUUKDZ-UHFFFAOYSA-J 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007788 liquid 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
- 238000002156 mixing Methods 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、気相反応法による窒化チタンの超微粉体の製
造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing ultrafine titanium nitride powder by a gas phase reaction method.
窒化チタンは７％副１点で耐熱性、耐食性に擾れておシ
、かつ高硬度であるだめ耐熱材料、研磨材料としての用
途があるほか、金属に近い電導性や超伝導性を示ずなど
の優れた電気的特性をもち、近年それらの利用開発が進
んでいる。Titanium nitride has excellent heat resistance and corrosion resistance at 7% sub-1 point, and is also highly hard, so it is used as a heat-resistant material and abrasive material, and it does not exhibit electrical conductivity or superconductivity close to that of metals. They have excellent electrical properties such as, and their use and development has progressed in recent years.
これらの利用の多くには、窒化チタンは焼結体として用
いられている。In many of these applications, titanium nitride is used as a sintered body.
焼結体の製造においては・、原料粉の特性が重要であっ
て、その粒度が小さく、かつ粒度分布が狭く、更に熱安
定性が大きいことが、焼結体の物性の向上に有効である
仁とが知られている。In the production of sintered bodies, the characteristics of the raw material powder are important, and its small particle size, narrow particle size distribution, and high thermal stability are effective in improving the physical properties of the sintered body. Jin is known.
従来、窒化チタ／の製造方法として幻、（１）金Ｆへチ
タン粉末全窒素又はアンモニア雰囲気で直接加熱窒化す
る方法。Conventionally, the method for producing titanium nitride has been phantom: (1) Direct heating and nitriding of titanium powder to gold F in a total nitrogen or ammonia atmosphere.
（２）水素化チタンを窒素又はアンモニアＷ ＩｌＮ気
中にて加熱する方法。(2) A method of heating titanium hydride in nitrogen or ammonia W IIN.
（３） ’Ｐｎ化チクチタン素の混合物を加熱下−て
窒素と反応させる方法。(3) A method in which a mixture of Pn-based titanium atoms is reacted with nitrogen under heating.
等が知られている。etc. are known.
しかしく１）の方法は、チタン粒子の内部まで窒化する
には高温度と長時間を要し、得られた窒化チタンの粒子
が大きいという欠点がある。（２）の方法は、水素化チ
タンが反応性に富み反応の制御が齢しく、操作上の危険
をとも々う欠点がある。また（３）の方ｉは、得られた
窒化チタンに’ＩｉＯ＋ ＴｌＣが固溶しやすく、純度
が低くなるという欠点がある。However, method 1) has the disadvantage that it requires high temperature and a long time to nitridate the inside of the titanium particles, and the obtained titanium nitride particles are large. The method (2) has the disadvantage that titanium hydride is highly reactive, the reaction control is slow, and there are operational risks. In addition, method (3) i has the disadvantage that 'IiO+TlC tends to form a solid solution in the obtained titanium nitride, resulting in low purity.
−刃高純度窒化チタンの製造方法としては、四塩化チタ
ンとアンモニアを高温で反応させる方法が知られている
が、超ｆ：Ｉ、粉すなわち１μｍ以下の窒化チタン粉を
製造するだめの詳細な方法は知られていない。しかして
特開昭３４−／！！０θを号公報には、四ハロゲン化チ
タンとアンモニアの反応によシ得られる含窒素ハロゲン
化チタンをアンモニアを含むガス加圧雰囲気下にて加熱
して窒化チタンを製造する方法が開示されており、′ま
た特開昭ｋＡ−７！；！１００７号公任には、前記公報
の方法における加圧下の加熱のほかに常圧下の加熱をも
含み、かつ約ｌＳθ℃〜り００℃の温度範囲を５θ℃／
分以上で加熱する方法が開示されている。これら公報の
方法によって、粒子径がＩＯｐｍ以下の窒化チタン粉が
得られるとしているが、ＩＯｐｍ以下の具体的な粒子径
については明らかにされておらず、また粒度分布につい
ても示されていない。- Blade A known method for producing high-purity titanium nitride is to react titanium tetrachloride and ammonia at high temperatures. The method is unknown. However, JP-A-34-/! ! Publication No. 0θ discloses a method for producing titanium nitride by heating nitrogen-containing titanium halide obtained by the reaction of titanium tetrahalide and ammonia in a pressurized gas atmosphere containing ammonia. ,' Also Tokkai Sho kA-7! ;! Publication No. 1007 includes heating under normal pressure in addition to the heating under pressure in the method of the above publication, and the temperature range from about 1Sθ℃ to 00℃ is 5θ℃/
A method of heating for more than 1 minute is disclosed. It is said that titanium nitride powder having a particle size of IOpm or less can be obtained by the methods in these publications, but the specific particle size of IOpm or less is not disclosed, nor is the particle size distribution disclosed.
これらの方法は、ともに含窒素ハロゲン化チタンを生成
させる工程と第一段の工程として分解工程があシ、また
、第一段目の工程はへ３〜３０気圧という高圧下で行な
う方法あるいは加熱のための昇温速度を規制した方法で
行なわれており、工業的生産方法として用いるには設備
面！操業面から複雑すぎるという欠点がある。Both of these methods involve a step of producing nitrogen-containing titanium halide and a decomposition step as the first step, and the first step is performed under high pressure of 3 to 30 atmospheres or by heating. It is carried out using a method that regulates the temperature increase rate, and it is difficult to use the equipment as an industrial production method! The drawback is that it is too complex from an operational standpoint.
更に、加藤他ｑ名は、ＴＩＣ／、 −ＮＨ３−Ｎ２−Ｎ
２系の気相反応による窒化チタン微粉体の合成を７００
°Ｃ〜１ｓｏｏ℃で行ない、反応条件がＴＩＮの粒ｍ１
粒度分布？原子比（Ｎ／’ｒ１）等に及ぼす影響を研究
し、その結果を報告している。（浩♀協会ｆ４Ｊｉ ｇ
３（？） ／９７！ ｒりｓ３）
これによれば、反応ガスの混合温（９）を７００″Ｃ以
上とすることにより、粒度が０．７μｍ以下で粒度分布
が狭い窒化チタンが得られるとしているが、Ｎ／Ｔ１は
へｌ〜へグであシ、非化学ｍ論性が非常に大きくなって
いるので、生成窒化チタンの熱安定性は高くない。まだ
上述したように使用するガスがｑ種類もあるため設備が
複雑になるという欠点がある。Furthermore, Kato et al. TIC/, -NH3-N2-N
Synthesis of titanium nitride fine powder by two-system gas phase reaction
The reaction conditions were TIN grain m1.
Particle size distribution? We are researching the effects on the atomic ratio (N/'r1), etc., and reporting the results. (Hiroshi Association f4Jig
3(?) /97! According to this, titanium nitride with a particle size of 0.7 μm or less and a narrow particle size distribution can be obtained by setting the reaction gas mixing temperature (9) to 700″C or higher, but N/T1 However, since the non-chemical properties are very large, the thermal stability of the titanium nitride produced is not high.As mentioned above, there are still q types of gases to be used, so the equipment The disadvantage is that it is complicated.
本発明は、四塩化チタンとアンモニアのみから直接窒化
チタンを製造する方法であって、従来法・による窒化チ
タン微粉よりも粒度が細かく、かつ粒度分布が狭く、更
にＮ／Ｔｉの原子比が化学量論量に近い値をもつ窒化チ
タンの超微粉を常圧下で製造することができる方法を提
供することを目的とするものである。The present invention is a method for directly producing titanium nitride from only titanium tetrachloride and ammonia, which has finer particle size and narrower particle size distribution than titanium nitride fine powder produced by conventional methods, and furthermore has a chemically low N/Ti atomic ratio. The object of the present invention is to provide a method capable of producing ultrafine titanium nitride powder having a value close to stoichiometric amount under normal pressure.
すなわち、本発明の要旨とするものは次のとおりである
。That is, the gist of the present invention is as follows.
四塩化チタンとアンモニアを常圧下において、１０００
℃〜／１１００″Ｃの範囲内の温度で反応させ、この生
成物を４００℃〜／ｌ／θｏ℃の範囲内の温度で不活゛
性ガス雰囲気中にて加熱することを特徴とする、気相反
応による窒化チタンの超微粉体の製造方法。Titanium tetrachloride and ammonia were heated at 1000 ml under normal pressure.
characterized in that the reaction is carried out at a temperature in the range from 400°C to /1100°C and the product is heated in an inert gas atmosphere at a temperature in the range from 400°C to /l/θo°C. A method for producing ultrafine titanium nitride powder by gas phase reaction.
以下、本発明の詳細を実験例に基づいて説明する。The details of the present invention will be explained below based on experimental examples.
実験に使用した装置は第１図に示したとおシである。す
なわち、コは石英製あるいはアルミナ製の反応管であっ
て、その直径は約Ｊｅｗ、長さは約／ＩＩであジ、その
ほぼ中央部には電気炉ｌが設けられておシ、その部分が
反応帯となっている。この反応管には、アンモニアを導
入するための導入管３と同心二重管６が反応帯まで挿入
されており、その同心二重管の内側の管は四塩化チタン
を導入するだめの導入管Ｓであシ、まだ外側の管はアル
ゴンを導入するだめの導入’ｆｙとなっている。その反
応管の反対側には、排気管７が設けられている。The apparatus used in the experiment is shown in Figure 1. That is, ``K'' is a reaction tube made of quartz or alumina, and its diameter is approximately Jew and the length is approximately /II. is the reaction zone. In this reaction tube, an introduction tube 3 for introducing ammonia and a concentric double tube 6 are inserted up to the reaction zone, and the inner tube of the concentric double tube is an introduction tube for introducing titanium tetrachloride. It is S, and the outer tube is still used for introducing argon. An exhaust pipe 7 is provided on the opposite side of the reaction tube.
まず、液体ＴｔＣ／４の、２（ＩＩ）りをｌθｓ′ｃで
加熱して気体ＴｔＣ４４を生成させ、これをアルゴンの
搬送気流によって同心二重管６の内側の管３を通して反
応管コ内に供給し、ｌθθθ°Ｃ〜／りθＯ″Ｃの設定
温度に保持しである、内径が３０ｍｍ、長さがＪＯＯｍ
ｍの反応帯に導入した。同心二重管６の外１■１１の管
ｙ内には、生成したＴ４Ｎが内側の管の出［Ｊ （＝Ｊ
近に析出づるのを妨けるため、包囲ガスとしてアルゴン
を導入した′。ＮＨ３は別の石英製導入管ＪをＪｊｎ
してｎｆ＋記反応帯に同時に供給した。First, 2(II) of liquid TtC/4 is heated at lθs'c to generate gas TtC44, which is introduced into the reaction tube through the inner tube 3 of the concentric double tube 6 using an argon carrier gas flow. The inner diameter is 30 mm and the length is JOOm.
m was introduced into the reaction zone. Outside the concentric double tube 6, inside the tube y of 1■11, the generated T4N is exposed to the inner tube [J
Argon was introduced as a surrounding gas to prevent precipitation in the vicinity. For NH3, connect another quartz introduction tube Jjn.
and simultaneously supplied to the nf+ reaction zone.
反応によって生成したＴｔＮ ｉｌ、副成しだＮＨ４Ｇ
ｇと共に反応帯の外側の室温部に析出した。この反応生
成物の混合物をアルゴン気流中あるいは真空下で加熱し
て、ＮＨ，Ｏｉを除去した。TtNil produced by the reaction, NH4G produced by the reaction
It precipitated along with g at room temperature outside the reaction zone. The reaction product mixture was heated in an argon stream or under vacuum to remove NH and Oi.
このようにして生成したＴ ＩＮｘの原子比Ｎ／Ｔｔ′
ｆ：調べたところ、１００θ〜／４１゜０°Ｃで生成し
たものは約へ１０であった。Atomic ratio N/Tt' of T INx produced in this way
f: Upon investigation, it was found that those produced at 100θ~/41°0°C were approximately 10°C.
続いて、前記のＴ１Ｃ１，とＮＨ３との反応で生成した
ＴｔＮよ、□。をアルゴン雰囲気中で種々の温度で７時
間加熱した結果、６θｏ°Ｃ未満ではＮ／Ｔ１比にほと
んど変化がなく、６θｏ°Ｃ以上になると可及的にＮ／
Ｔｔ比は減少し、９θｏ°Ｃ以上でほぼ八。−となシは
ぼ一定となった。Next, TtN produced by the reaction between T1C1 and NH3 mentioned above, □. As a result of heating at various temperatures in an argon atmosphere for 7 hours, there was almost no change in the N/T1 ratio below 6θo°C, and as much as possible at temperatures above 6θo°C.
The Tt ratio decreases and is approximately 8 above 9θo°C. - Tonashi has become more or less constant.
次に／Ｑθθ°Ｃ以上で生成したＴｉＮｘを可、子顕微
鏡によって粒度を測定したところ、／コθｏ′ｃで生成
したものの粒度はｏ、ｉ〜０．−μｍであり、同じく７
３００℃のもので０．０！； −０，／ ｐｍ 、 ／
１１００ ℃のものでθ、θｌ〜θ、θりμｍであった
。Next, when the particle size of the TiNx produced at /Qθθ°C or higher was measured using a submicroscope, the particle size of the TiNx produced at /Qθo'c was o, i ~ 0. − μm, which is also 7
0.0 at 300℃! ; −0, / pm, /
At 1100°C, the values were θ, θ1 to θ, and θμm.
これから分かるように、ＴｌＮｘの粒度は高温になるに
従って細かく、かつ粒度分布も狭くなっている。更にほ
ぼ球状の粒子であシ、このような微粉は＼前述のように
焼結体用原料粉とじて好ましいものである。As can be seen from this, the particle size of TINx becomes finer and the particle size distribution becomes narrower as the temperature increases. Further, the particles are approximately spherical in shape, and such fine powder is preferable as a raw material powder for a sintered body as described above.
次に、本発明において四塩化チタンとアンモニアの反応
温度を１０００℃〜／グ００℃の範囲に限定した理由を
説明する。Next, the reason why the reaction temperature of titanium tetrachloride and ammonia is limited to a range of 1000°C to 00°C in the present invention will be explained.
まず、反応温度が７θｏ℃より低い温度ではＴｚＮｘの
他に含窒素塩化チタン、四塩化チタン−アンモニア附加
物が生成するため不適当である。７００”Ｃ以−ヒにな
ると反応生成物はＴｉＮｘのみになるが、Ｎ／Ｔｔ比が
大きく、更に生成ＴｉＮｘの粒度が比較的大きい。それ
に対して７０００℃以上の反応温度で生成したものは後
述するごとく粒度が小さく、かつ均一である。また７９
００℃を超えるとＴｔＮ父ｔま分解しやすくなるため遅
応温度範囲は１ｏｏｏ℃〜／１１００℃とした。First, a reaction temperature lower than 7θoC is unsuitable because nitrogen-containing titanium chloride and titanium tetrachloride-ammonia adducts are produced in addition to TzNx. At 700"C or higher, the reaction product is only TiNx, but the N/Tt ratio is large and the particle size of the TiNx produced is relatively large.On the other hand, those produced at a reaction temperature of 7000"C or higher will be described later. As expected, the particle size is small and uniform.79
If the temperature exceeds 00°C, TtN tends to decompose, so the slow reaction temperature range was set to 100°C to 1100°C.
次いで反応生成物を不活性ガス８′囲気中で加熱する温
度をＡＯＯ′Ｃ〜／’１００℃に限定したのは、前記実
験結果によると、６θｏ ’ｃ−ｌＦ−満てはｉ−１／
Ｔｉ比にほとんど変化がなく、９００℃以上でＮ／Ｔｉ
比はほぼ一定となるが、前記のようにｉｑθ０℃を超え
るとＴｔＮｘは分解しやすくなるためであシ、なかでも
ｑｏｏ℃〜１０００・℃が好適である。Next, the temperature at which the reaction product was heated in an inert gas atmosphere was limited to AOO'C~/'100°C because, according to the above experimental results, 6θo'c−1F− is less than i−1/
There is almost no change in the Ti ratio, and the N/Ti ratio increases above 900°C.
Although the ratio is approximately constant, as mentioned above, if iqθ exceeds 0°C, TtNx becomes easy to decompose, so qoo°C to 1000°C is particularly preferable.
以上述べてきたとおり、本発明によれば、高純・度であ
って、粒度が細かく、かつ粒（９）分布が狭く、更に原
子比がほぼ化学量論量であって熱安定性の高イＴｔＮを
得ることができる。As described above, according to the present invention, the present invention has high purity and purity, fine particle size, narrow particle (9) distribution, almost stoichiometric atomic ratio, and high thermal stability. It is possible to obtain a good TtN.
第１図は、本発明の実醗例に使用した装置を示す図であ
る。
１・・・電気炉、コ・・・反応管、３・・・アンモニア
導入管、ダ・・・アルゴン導入管、３・・・四塩化チタ
ン導入管、６・・・同心二重管、り・・・排気管。
特許出願人 日本重化学工業株式会社
代理人弁理士 村 １） 政 治FIG. 1 is a diagram showing an apparatus used in a practical example of the present invention. 1... Electric furnace, C... Reaction tube, 3... Ammonia introduction tube, D... Argon introduction tube, 3... Titanium tetrachloride introduction tube, 6... Concentric double tube, R ···Exhaust pipe. Patent applicant: Japan Heavy and Chemical Industry Co., Ltd. Representative Patent Attorney Mura 1) Politics
Claims (1)
０℃〜／Ｖθθ°Ｃの範囲内の温度で反応させ、この生
成物をＡＯＯ℃〜／／Ｉθθ℃の範囲内の温度で、不活
性ガス雰囲気中にて加熱することを特徴とする、気相反
応法による窒化チタンの超微粉体の製造方法。1. Titanium tetrachloride and ammonia are heated to 100% under normal pressure.
The reaction is carried out at a temperature in the range of 0°C to /Vθθ°C, and the product is heated in an inert gas atmosphere at a temperature in the range of AOO°C to /Iθθ°C. A method for producing ultrafine titanium nitride powder using a phase reaction method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18678982A JPS5976802A (en) | 1982-10-26 | 1982-10-26 | Manufacture of hyperfine powder of titanium nitride by vapor phase reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18678982A JPS5976802A (en) | 1982-10-26 | 1982-10-26 | Manufacture of hyperfine powder of titanium nitride by vapor phase reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5976802A true JPS5976802A (en) | 1984-05-02 |
| JPS6117764B2 JPS6117764B2 (en) | 1986-05-09 |
Family
ID=16194611
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18678982A Granted JPS5976802A (en) | 1982-10-26 | 1982-10-26 | Manufacture of hyperfine powder of titanium nitride by vapor phase reaction |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5976802A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5002646A (en) * | 1988-04-23 | 1991-03-26 | Tioxide Group Plc | Method for making titanium nitride |
| US10954166B2 (en) | 2015-03-09 | 2021-03-23 | Sumitomo Electric Industries, Ltd. | Ceramic powder and boron nitride sintered material |
-
1982
- 1982-10-26 JP JP18678982A patent/JPS5976802A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5002646A (en) * | 1988-04-23 | 1991-03-26 | Tioxide Group Plc | Method for making titanium nitride |
| US10954166B2 (en) | 2015-03-09 | 2021-03-23 | Sumitomo Electric Industries, Ltd. | Ceramic powder and boron nitride sintered material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6117764B2 (en) | 1986-05-09 |
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