JPH04317413A - Production of titanium suboxide - Google Patents
Production of titanium suboxideInfo
- Publication number
- JPH04317413A JPH04317413A JP11231891A JP11231891A JPH04317413A JP H04317413 A JPH04317413 A JP H04317413A JP 11231891 A JP11231891 A JP 11231891A JP 11231891 A JP11231891 A JP 11231891A JP H04317413 A JPH04317413 A JP H04317413A
- Authority
- JP
- Japan
- Prior art keywords
- titanium
- titanium dioxide
- vacuum
- suboxide
- melting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 31
- 239000010936 titanium Substances 0.000 title claims abstract description 31
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 33
- -1 titanium hydride Chemical compound 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 abstract description 14
- 238000007740 vapor deposition Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 12
- 238000002844 melting Methods 0.000 abstract description 11
- 230000008018 melting Effects 0.000 abstract description 11
- 239000000843 powder Substances 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 5
- 229910009815 Ti3O5 Inorganic materials 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 3
- 238000010309 melting process Methods 0.000 abstract description 2
- 239000008188 pellet Substances 0.000 description 11
- 238000000151 deposition Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 230000008021 deposition Effects 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 229910009848 Ti4O7 Inorganic materials 0.000 description 3
- 229910009870 Ti5O9 Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 150000003608 titanium Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、有色顔料、導電性フィ
ラー、蒸着材等に用いる亜酸化チタンの製造方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing titanium suboxide used for colored pigments, conductive fillers, vapor deposition materials, and the like.
【０００２】0002
【従来の技術】亜酸化チタンは、二酸化チタンとは異な
り還元反応によって茶褐色、灰色、黒紫色あるいは黒色
など多様な色調を現出するうえに、良好な導電性能を有
するため有色顔料や各種材料の導電性フィラーとして汎
用されているが、近時、光学系、オプトエレクトロニク
ス等の分野で基材面に二酸化チタンの薄膜を形成するた
めの蒸着材料として利用が図られている。[Prior Art] Unlike titanium dioxide, titanium suboxide produces various colors such as brownish-brown, gray, black-purple, or black through a reduction reaction, and also has good electrical conductivity, which makes it suitable for use as colored pigments and various materials. Although it is commonly used as a conductive filler, recently it has been used as a vapor deposition material for forming a thin film of titanium dioxide on a substrate surface in fields such as optical systems and optoelectronics.
【０００３】従来、亜酸化チタンを製造する手段には、
二酸化チタンを水素またはアンモニア等のガスで高温還
元する方法（特公昭５９−５０６０４ 号公報、特開昭
５７−２０５３２２号公報） 、二酸化チタンと金属チ
タンの混合物を真空中または還元雰囲気中で加熱する方
法（特開昭４９−５４３２号公報） が典型的な技術と
して知られている。これらの方法は固相−気相系あるい
は固相−固相系の原料組成による還元反応を利用するも
ので、得れる亜酸化チタンは一般にＴｉＯ、Ｔｉ２ Ｏ
３ 、Ｔｉ３ Ｏ５ 、Ｔｉ４ Ｏ ７、Ｔｉ５ Ｏ９
の組成を有し、いずれも焼結体である。Conventionally, methods for producing titanium suboxide include:
A method of reducing titanium dioxide at high temperature with a gas such as hydrogen or ammonia (Japanese Patent Publication No. 59-50604, Japanese Patent Application Laid-open No. 57-205322), heating a mixture of titanium dioxide and metallic titanium in a vacuum or in a reducing atmosphere. The method (Japanese Unexamined Patent Publication No. 49-5432) is known as a typical technique. These methods utilize a reduction reaction depending on the raw material composition of a solid phase-gas phase system or a solid phase-solid phase system, and the obtained titanium suboxide is generally TiO, Ti2O
3, Ti3O5, Ti4O7, Ti5O9
Both are sintered bodies.
【０００４】亜酸化チタン蒸着材による二酸化チタンの
被膜は、抵抗加熱、電子ビーム加熱等で溶解したのち基
材面に真空蒸着する方法で形成されるが、この際、前記
のＴｉＯやＴｉ２ Ｏ３ はガス吸収作用を起し、また
Ｔｉ４ Ｏ ７やＴｉ５ Ｏ９ は逆にガス発生作用を
起して真空槽内の雰囲気を一定に保ち得ない。その点、
Ｔｉ３ Ｏ５ は減圧、高温雰囲気下で極めて安定であ
るが、前記の従来技術で製造されたＴｉ３ Ｏ５ で表
わされる亜酸化チタン焼結体（以下、単に亜酸化チタン
という。）を蒸着材とした場合には、真空加熱状態での
スプラッシュ現象が著しく多発する。スプラッシュ現象
が多く発生すると、基材面への均一な蒸着が阻害される
ばかりでなく、蒸着装置に蒸着物が付着したり、電子銃
フィラメントが酸化変質する等のトラブルを招く。この
現象を避けるために、スプラッシュが鎮静化してから膜
付け操作をおこなうこともできるが、この場合には時間
のロスが大きくなる。
従って、二酸化チタン形成薄膜材料に求められる要件は
、ガス発生やガス吸収を起さず、かつスプラッシュ現象
を生起せず、不純物の少ないものが好ましいとされてい
る。[0004] A titanium dioxide film made of a titanium suboxide vapor deposition material is formed by melting it by resistance heating, electron beam heating, etc., and then vacuum vapor depositing it on the substrate surface. Ti4O7 and Ti5O9 cause a gas-absorbing effect, and conversely, Ti4O7 and Ti5O9 cause a gas-generating effect, making it impossible to maintain a constant atmosphere in the vacuum chamber. That point,
Ti3 O5 is extremely stable under reduced pressure and high temperature atmosphere, but when a titanium suboxide sintered body (hereinafter simply referred to as titanium suboxide) represented by Ti3 O5 manufactured by the above-mentioned conventional technique is used as a vapor deposition material. Splash phenomena occur extremely frequently under vacuum heating conditions. If many splash phenomena occur, not only will uniform vapor deposition on the substrate surface be inhibited, but it will also cause problems such as deposition material adhering to the vapor deposition device and oxidation deterioration of the electron gun filament. In order to avoid this phenomenon, it is possible to carry out the film deposition operation after the splash has subsided, but in this case there is a large loss of time. Therefore, the requirements for a titanium dioxide-forming thin film material are preferably one that does not generate or absorb gas, does not cause a splash phenomenon, and has few impurities.
【０００５】このような問題を解消するために有効な亜
酸化チタンの製造方法として、粒度８０μｍ 以下の水
素化チタン粉末と二酸化チタンとの混合物を ７００〜
１６００℃の温度域において真空または不活性ガス雰囲
気下で加熱焼成する技術が、本出願人によって開発され
ている（特開平１−２９０５２９号公報） 。[0005] As an effective method for producing titanium suboxide to solve these problems, a mixture of titanium hydride powder with a particle size of 80 μm or less and titanium dioxide is
The present applicant has developed a technique of heating and firing in a temperature range of 1600° C. in a vacuum or an inert gas atmosphere (Japanese Patent Laid-Open No. 1-290529).
【０００６】[0006]
【発明が解決しようとする課題】該先行技術によれば、
製造される亜酸化チタンが蒸着に好適な粒子状態を呈し
ており、またガス成分や不純物の含有量を効果的に低減
化されているため、スプラッシュやアウトガスの発生は
従来技術に比べてかなり減少させることが可能となる。
しかしながら、この製法で得られる亜酸化チタンは不純
物も少なくガス発生もないが、スプラッシュ現象に対す
る防止効果については十分とはいえない。[Problem to be Solved by the Invention] According to the prior art,
The produced titanium suboxide has a particle state suitable for vapor deposition, and the content of gas components and impurities is effectively reduced, so the generation of splash and outgas is significantly reduced compared to conventional technology. It becomes possible to do so. However, although the titanium suboxide obtained by this manufacturing method has few impurities and does not generate gas, it cannot be said to be sufficiently effective in preventing splash phenomena.
【０００７】本発明は、二酸化チタンを還元・焼結して
亜酸化チタンを得るというこれまでの製造技術とは全く
異なるプロセスによって蒸着材用亜酸化チタンを製造す
る方法を対象とするもので、その目的は蒸着時の真空加
熱段階におけるスプラッシュ現象を効果的に低減化し得
る蒸着用亜酸化チタンの製造方法を提供することにある
。The present invention is directed to a method of producing titanium suboxide for vapor deposition material by a process completely different from the conventional production technology of reducing and sintering titanium dioxide to obtain titanium suboxide. The purpose is to provide a method for producing titanium suboxide for deposition, which can effectively reduce the splash phenomenon during the vacuum heating step during deposition.
【０００８】[0008]
【課題を解決するための手段】上記の目的を達成するた
めの本発明による蒸着材用亜酸化チタンの製造方法は、
二酸化チタンまたは水素化チタンと二酸化チタンの混合
物を、真空雰囲気下で二酸化チタンが溶解する温度以上
に加熱することを構成上の特徴とするものである。[Means for Solving the Problems] A method for producing titanium suboxide for vapor deposition material according to the present invention to achieve the above object is as follows:
The structural feature is that titanium dioxide or a mixture of titanium hydride and titanium dioxide is heated in a vacuum atmosphere to a temperature higher than that at which titanium dioxide dissolves.
【０００９】本発明の原料となる二酸化チタンは、硫酸
法、塩素法のいずれの方法で製造されたものでもよく、
また結晶型はアナターゼ型、ルチル型、ブルカイト型の
いずれであっても差し支えない。該二酸化チタンは粉末
として使用されるが、その粒度には特に制約はない。二
酸化チタンと共用する他方の原料となる水素化チタンも
粉末として使用されるが、この場合の粉末化は、粒状の
水素化チタンを水素雰囲気中で ４００〜７００ ℃に
加熱して易粉砕状態に転化したのち、ボールミルまたは
振動ミル等で粉砕することが好ましい。Titanium dioxide, which is the raw material of the present invention, may be produced by either the sulfuric acid method or the chlorine method.
Further, the crystal type may be anatase type, rutile type, or brookite type. Although the titanium dioxide is used as a powder, there are no particular restrictions on its particle size. Titanium hydride, which is the other raw material used in common with titanium dioxide, is also used in the form of powder, but in this case, granular titanium hydride is heated to 400 to 700 °C in a hydrogen atmosphere to make it easily pulverized. After conversion, it is preferable to pulverize with a ball mill, a vibration mill, or the like.
【００１０】上記の原料は、二酸化チタン単独または水
素化チタンと二酸化チタンの混合物とし、予めペレット
状に成形したのち溶解工程にかけられる。ペレット成形
は、通常の油圧式または機械式のプレス装置を用いてお
こなわれるが、金型のかじり防止と離型性を良くするた
め必要に応じて適宜なバインダー成分を添加してもかま
わない。水素化チタンと二酸化チタンを混合して原料と
する際には、配合割合を重量比で８〜１０：１の範囲に
設定し、乾式もしくは湿式法によって混合される。[0010] The above raw material is titanium dioxide alone or a mixture of titanium hydride and titanium dioxide, which is formed into pellets in advance and then subjected to a melting process. Pellet molding is carried out using an ordinary hydraulic or mechanical press device, but an appropriate binder component may be added as necessary to prevent galling of the mold and improve mold release properties. When titanium hydride and titanium dioxide are mixed to form a raw material, the mixing ratio is set in a range of 8 to 10:1 by weight, and the mixture is carried out by a dry or wet method.
【００１１】溶解工程は、原料ペレットを真空雰囲気に
保持された加熱装置、好ましくは電気炉に移し、二酸化
チタンが溶解する温度以上に加熱することによっておこ
なわれる。好適な溶解条件は、加熱時の雰囲気を１Ｔｏ
ｒｒ以下の真空状態に保ち、温度を１８００℃以上の範
囲に設定することである。この真空度において、加熱温
度を１８００℃未満にすると二酸化チタンの溶解が円滑
に進行せず、他方、２０００℃を越えると生成した亜酸
化チタンが蒸発して収率が低下する。[0011] The melting step is carried out by transferring the raw material pellets to a heating device maintained in a vacuum atmosphere, preferably an electric furnace, and heating them to a temperature higher than the temperature at which titanium dioxide melts. Suitable melting conditions include a heating atmosphere of 1To
The purpose is to maintain a vacuum state below rr and set the temperature in a range of 1800°C or above. At this degree of vacuum, if the heating temperature is less than 1800°C, the dissolution of titanium dioxide will not proceed smoothly, while if it exceeds 2000°C, the produced titanium suboxide will evaporate and the yield will decrease.
【００１２】溶解後は、真空または不活性ガス雰囲気中
で冷却し、生成した亜酸化チタンを製品として取り出す
。After melting, it is cooled in a vacuum or in an inert gas atmosphere, and the produced titanium suboxide is taken out as a product.
【００１３】[0013]
【作用】本発明によれば、原料となる二酸化チタンまた
は水素化チタンと酸化チタンの混合物を単に真空雰囲気
下で溶解することによりＴｉ３ Ｏ５ を主体とする低
次酸化形態の亜酸化チタンに転化する。この際、溶解工
程が真空雰囲気下でおこなわれるから、二酸化チタン及
び水素化チタン中に含まれている不純物成分は効果的に
揮散除去される。[Operation] According to the present invention, the raw material titanium dioxide or a mixture of titanium hydride and titanium oxide is simply melted in a vacuum atmosphere to convert it into titanium suboxide in a lower oxidation form mainly consisting of Ti3O5. . At this time, since the melting step is performed under a vacuum atmosphere, impurity components contained in titanium dioxide and titanium hydride are effectively volatilized and removed.
【００１４】このような作用を介して、蒸着時の真空加
熱段階でスプラッシュ現象を生じない高品質の亜酸化チ
タンを製造することが可能となる。Through this effect, it is possible to produce high quality titanium suboxide that does not cause a splash phenomenon during the vacuum heating stage during vapor deposition.
【００１５】[0015]
【実施例】以下、本発明の実施例を比較例と対比して説
明する。
実施例１
二酸化チタン粉末を機械式成形プレスを用いて成形し、
直径１０ｍｍ、厚さ４ｍｍの錠剤形ペレットとした。つ
いで、ペレットを耐熱ルツボに入れて電気炉に移し、炉
内を１Ｔｏｒｒ以下の真空に保持しながら１８００℃の
温度で８時間加熱してペレットを溶解し、そのまま炉冷
した。[Examples] Examples of the present invention will be explained below in comparison with comparative examples. Example 1 Titanium dioxide powder was molded using a mechanical molding press,
It was made into a tablet-shaped pellet with a diameter of 10 mm and a thickness of 4 mm. Next, the pellets were placed in a heat-resistant crucible, transferred to an electric furnace, heated at a temperature of 1800° C. for 8 hours while maintaining the inside of the furnace in a vacuum of 1 Torr or less to melt the pellets, and then cooled in the furnace as it was.
【００１６】得られた生成物は赤紫色を呈しており、そ
の化合物組成を粉末Ｘ線回折法で測定した結果、Ｔｉ３
Ｏ５ であることが確認された。この亜酸化チタンを
ＥＢ溶解炉で溶解し、真空下でスプラッシュの状況を観
察したところ、スプラッシュ現象は殆ど認められなかっ
た。The obtained product had a reddish-purple color, and its compound composition was measured by powder X-ray diffraction, and it was found that Ti3
It was confirmed that it was O5. When this titanium suboxide was melted in an EB melting furnace and the state of splash was observed under vacuum, almost no splash phenomenon was observed.
【００１７】実施例２
粒度４５μｍ 以下の水素化チタン粉末と二酸化チタン
粉末を重量比で９：１の割合で配合し、ボールミルによ
り１２時間混合処理を施した。この混合粉末を機械式成
形プレスで成形し、直径１０ｍｍ、厚さ４ｍｍの錠剤形
ペレットとした。ついで、ペレットを耐熱ルツボに入れ
て電気炉に移し、炉内を１Ｔｏｒｒ以下の真空雰囲気に
保持しながら１８５０℃の温度で１５分間加熱してペレ
ットを溶解し、そのまま炉冷した。Example 2 Titanium hydride powder and titanium dioxide powder having a particle size of 45 μm or less were mixed at a weight ratio of 9:1, and mixed for 12 hours using a ball mill. This mixed powder was molded using a mechanical molding press to form tablet-shaped pellets with a diameter of 10 mm and a thickness of 4 mm. Next, the pellets were placed in a heat-resistant crucible, transferred to an electric furnace, heated at a temperature of 1850° C. for 15 minutes while maintaining the inside of the furnace in a vacuum atmosphere of 1 Torr or less to melt the pellets, and then cooled in the furnace.
【００１８】得られた生成物は赤紫色を呈しており、そ
の化合物組成を粉末Ｘ線回折法で測定した結果、Ｔｉ３
Ｏ５ であることが確認された。この亜酸化チタンを
ＥＢ溶解炉で溶解し、真空下でスプラッシュの状況を観
察したところ、スプラッシュ現象は殆ど認められなかっ
た。The obtained product had a reddish-purple color, and its compound composition was measured by powder X-ray diffraction method. As a result, Ti3
It was confirmed that it was O5. When this titanium suboxide was melted in an EB melting furnace and the state of splash was observed under vacuum, almost no splash phenomenon was observed.
【００１９】比較例１
粒度４５μｍ 以下の水素化チタン粉末５５５ｇと二酸
化チタン粉末４４４５ｇ を配合し、乾式混合機で１２
時間混合したのち、機械式成形プレスを用いて直径１０
ｍｍ、厚さ４ｍｍの錠剤形ペレットに成形した。ついで
、このペレットを真空雰囲気炉に入れ、１２２０℃の温
度で８時間加熱して還元焼成した。得られた焼結体は黒
紫色を呈しており、その化合物組成を粉末Ｘ線回折法で
測定した結果、Ｔｉ３ Ｏ５ であることが確認された
。この亜酸化チタンをＥＢ溶解炉で溶解し、真空下でス
プラッシュの状況を観察したところ、スプラッシュ現象
が多く発生した。Comparative Example 1 555 g of titanium hydride powder with a particle size of 45 μm or less and 4445 g of titanium dioxide powder were blended and mixed in a dry mixer for 12 hours.
After mixing for a period of time, a diameter of 10 mm was formed using a mechanical forming press.
It was molded into tablet-shaped pellets with a thickness of 4 mm and a thickness of 4 mm. Next, the pellets were placed in a vacuum atmosphere furnace and heated at a temperature of 1220° C. for 8 hours to perform reduction firing. The obtained sintered body had a blackish-purple color, and its compound composition was measured by powder X-ray diffraction, and as a result, it was confirmed to be Ti3O5. When this titanium suboxide was melted in an EB melting furnace and the state of splash was observed under vacuum, many splash phenomena occurred.
【００２０】[0020]
【発明の効果】以上のとおり、本発明によれば従来の還
元焼結法とは異なり、二酸化チタンまたは水素化チタン
と二酸化チタンの混合物を単に真空雰囲気下で溶解処理
することにより蒸着時の真空加熱過程で発生するスプラ
ッシュ現象を効果的に低減化することができる亜酸化チ
タンを製造することができる。したがって、常に円滑に
高品質のチタン系蒸着薄膜を形成するための蒸着材を生
産供給することが可能となる。As described above, according to the present invention, unlike the conventional reduction sintering method, titanium dioxide or a mixture of titanium hydride and titanium dioxide is simply melted in a vacuum atmosphere, thereby reducing the vacuum during vapor deposition. It is possible to produce titanium suboxide that can effectively reduce the splash phenomenon that occurs during the heating process. Therefore, it is possible to always produce and supply a vapor deposition material for smoothly forming a high quality titanium-based vapor deposited thin film.
Claims (2)
酸化チタンの混合物を、真空雰囲気下で二酸化チタンが
溶解する温度以上に加熱することを特徴とする亜酸化チ
タンの製造方法。1. A method for producing titanium suboxide, which comprises heating titanium dioxide or a mixture of titanium hydride and titanium dioxide in a vacuum atmosphere to a temperature higher than the temperature at which titanium dioxide dissolves.
空状態に保持し、温度を１８００℃以上に設定する請求
項１記載の亜酸化チタンの製造方法。2. The method for producing titanium suboxide according to claim 1, wherein the atmosphere during heating is maintained in a vacuum state of 1 Torr or less, and the temperature is set at 1800° C. or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11231891A JPH04317413A (en) | 1991-04-16 | 1991-04-16 | Production of titanium suboxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11231891A JPH04317413A (en) | 1991-04-16 | 1991-04-16 | Production of titanium suboxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04317413A true JPH04317413A (en) | 1992-11-09 |
Family
ID=14583671
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11231891A Pending JPH04317413A (en) | 1991-04-16 | 1991-04-16 | Production of titanium suboxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04317413A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0601761A1 (en) * | 1992-11-30 | 1994-06-15 | Shiseido Company Limited | Manufacturing method of pigment including lower titanium oxide |
| JP2010024111A (en) * | 2008-07-23 | 2010-02-04 | Toho Titanium Co Ltd | Method for producing titanium suboxide |
-
1991
- 1991-04-16 JP JP11231891A patent/JPH04317413A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0601761A1 (en) * | 1992-11-30 | 1994-06-15 | Shiseido Company Limited | Manufacturing method of pigment including lower titanium oxide |
| JP2010024111A (en) * | 2008-07-23 | 2010-02-04 | Toho Titanium Co Ltd | Method for producing titanium suboxide |
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