JPH02271919A - Production of fine powder of titanium carbide - Google Patents
Production of fine powder of titanium carbideInfo
- Publication number
- JPH02271919A JPH02271919A JP1090376A JP9037689A JPH02271919A JP H02271919 A JPH02271919 A JP H02271919A JP 1090376 A JP1090376 A JP 1090376A JP 9037689 A JP9037689 A JP 9037689A JP H02271919 A JPH02271919 A JP H02271919A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- particle size
- average particle
- titanium oxide
- tio2
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 29
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 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 37
- 239000002245 particle Substances 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 9
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract description 6
- 229910003481 amorphous carbon Inorganic materials 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 239000006232 furnace black Substances 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- 239000010439 graphite Substances 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract 2
- 239000000463 material Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 18
- 239000002994 raw material Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 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
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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、高融点、高強度、高硬度、高耐食の特徴を備
え、切削工具等として有用な炭化チタン焼結体の原料微
粉末の製造方法に関する。Detailed Description of the Invention [Industrial Application Field] The present invention is directed to a fine powder raw material for a titanium carbide sintered body, which has the characteristics of a high melting point, high strength, high hardness, and high corrosion resistance, and is useful as a cutting tool, etc. Regarding the manufacturing method.
［従来技術とその解決しようとする課題］従来、炭化チ
タンの製造法としては、チタンと炭素を直接反応させる
方法がよく知られている。[Prior Art and Problems to be Solved] Conventionally, as a method for producing titanium carbide, a method of directly reacting titanium and carbon is well known.
しかし、この反応は、使用する原料が高価である上、発
熱反応であるので得られる炭化チタンの粉末は粒子径が
大きいものとなるという問題点がある。However, this reaction has problems in that the raw materials used are expensive and, since it is an exothermic reaction, the resulting titanium carbide powder has a large particle size.
また、微細な粉末を得るためには、四塩化チタンと炭化
水素等の反応による所謂気相法による方法があるが、上
記方法は原料が高価である上大量生産が簡単でなく得ら
れる粉末が高価になり、工業的な方法とは言えない。In addition, in order to obtain fine powder, there is a method using the so-called gas phase method by reacting titanium tetrachloride with hydrocarbons, etc., but the above method requires expensive raw materials and is difficult to mass produce, making it difficult to obtain powder. It is expensive and cannot be called an industrial method.
さらに、より工業的な製造法として酸化チタンを炭素と
反応させる方法が知られているが、通常の方法ではサブ
ミクロン級の粉末を製造するのは難しく、未だに適当な
方法がない。Furthermore, a method of reacting titanium oxide with carbon is known as a more industrial production method, but it is difficult to produce submicron-sized powder using normal methods, and there is still no suitable method.
炭化チタンは硬度が高く、粉砕によっても微粉化するこ
とは非常に困難であり、前記した各種物性を活かして良
好な焼結体を得るためには、均一かつ微細な炭化チタン
粉末が要望されているのにもかかわらず、上述したよう
に種々の方法によっても工業的に容易に微粉末を得る製
造法がないのが現状である。Titanium carbide has high hardness and is extremely difficult to pulverize even by pulverization. In order to obtain a good sintered body by taking advantage of the various physical properties mentioned above, uniform and fine titanium carbide powder is required. However, as mentioned above, there is currently no manufacturing method for easily obtaining fine powder industrially using the various methods described above.
［課題を解決するための手段］
本発明者らはこのような現状に鑑み、上記問題点を解決
するために鋭意検討を行った結果、原料の一部に極めて
微細な酸化チタンを添加することにより、より微細な炭
化チタン粉末が製造できることを見い出し本発明に到達
したものである。[Means for Solving the Problems] In view of the current situation, the present inventors conducted intensive studies to solve the above problems, and as a result, they decided to add extremely fine titanium oxide to some of the raw materials. The present invention was achieved by discovering that finer titanium carbide powder can be produced by the above method.
すなわち本発明は、酸化チタンと炭素を非酸化性雰囲気
下で１３００〜１８００℃の温度で焼成することにより
炭化チタンを得る方法において、平均粒径０．１〜５μ
ｍの酸化チタン１００重量部に対して、添加剤として平
均粒径０．０５μｍ以下の酸化チタンを０．０５〜３０
重量部添加することを特徴とする炭化チタン微粉末の製
造方法である。That is, the present invention provides a method for obtaining titanium carbide by firing titanium oxide and carbon at a temperature of 1,300 to 1,800°C in a non-oxidizing atmosphere.
0.05 to 30 parts by weight of titanium oxide with an average particle size of 0.05 μm or less as an additive to 100 parts by weight of titanium oxide.
This is a method for producing fine titanium carbide powder, characterized in that part by weight of titanium carbide is added.
本発明では主たる原料粉末としての酸化チタンおよび炭
素にさらに、より微細な酸化チタンを添加して反応に供
することにより微細な炭化チタン粉末を製造しようとす
るものである。The present invention aims to produce fine titanium carbide powder by adding finer titanium oxide to titanium oxide and carbon as the main raw material powders and subjecting the mixture to a reaction.
添加剤としての酸化チタンは、主原料の酸化チタンに比
較してかなり微細な粉末である必要があり、焼結体原料
として良好な粉末となる０、６μｍ程度以下の炭化チタ
ン粉末を得るためには、０．０５μｍ以下の微細酸化チ
タンが好ましく、該粉末は四塩化チタンの酸化分解等の
気相法により得られたものを使用することができる。Titanium oxide as an additive needs to be a considerably finer powder than the main raw material titanium oxide, and in order to obtain titanium carbide powder of about 0.6 μm or less, which is a good powder as a raw material for sintered bodies. is preferably a fine titanium oxide powder of 0.05 μm or less, and the powder obtained by a gas phase method such as oxidative decomposition of titanium tetrachloride can be used.
この添加剤として用いる酸化チタンの添加量は主たる原
料の酸化チタン１００ ｆ！量部に対し、０．０５〜３
０重量部の範囲が好ましく 、０．０５〜１０重量部の
範囲がより好ましい、０．０５重量部より少ない場合は
添加剤の効果による生成炭化チタンの微細化の程度が十
分でなく、一方３０重量部を越えた場合、微細化の効果
は増加はあまり期待できず経済的でない。The amount of titanium oxide used as this additive is 100 f! of titanium oxide, the main raw material. 0.05 to 3 parts
The range of 0 parts by weight is preferable, and the range of 0.05 to 10 parts by weight is more preferable. If the amount exceeds parts by weight, the effect of refinement cannot be expected to increase much and is not economical.
本発明において、主たる原料として用いる酸化チタン粉
末としては粒子径の小さいもののほうが反応速度が大と
なり、また生成する粒子自体も当然微細となるので好ま
しいが、０，１μｍ以下の酸化チタンは高価であり、ま
た上記したように微細な酸化チタンを添加することによ
り十分微細化の効果は上がるので、０．１〜５μｍ程度
の酸化チタンが好ましい、好ましい酸化チタンの粒子径
の上限を５μｍとしたのは、それより大きい場合は主反
応の反応速度が小さくなり、反応時間がかかりすぎるた
めである。In the present invention, the titanium oxide powder used as the main raw material is preferably one with a smaller particle size because the reaction rate is faster and the particles produced are naturally finer, but titanium oxide with a size of 0.1 μm or less is expensive. Also, as mentioned above, adding fine titanium oxide can sufficiently increase the effect of finer particles, so titanium oxide of about 0.1 to 5 μm is preferable, and the upper limit of the preferred titanium oxide particle size is set to 5 μm. , if it is larger than that, the reaction rate of the main reaction will be low and the reaction time will be too long.
次に原料となる炭素は、ファーネスブラック、アセチレ
ンブラック、ランプブランク等の無定形の炭素粉末や単
糖、多糖類等の水溶性炭水化物やタール、ピンチ等の難
溶性油脂類等が挙げられ、その添加量は全酸化チタンに
対して４０重量部以上７０重量部以下が好ましい。Next, the raw material carbon includes amorphous carbon powder such as furnace black, acetylene black, and lamp blank, water-soluble carbohydrates such as monosaccharides and polysaccharides, and sparingly soluble oils and fats such as tar and pinch. The amount added is preferably 40 parts by weight or more and 70 parts by weight or less based on the total titanium oxide.
本発明において、添加剤としての酸化チタンが生成する
炭化チタンの微細化にどのように寄与しているかは明ら
かではないが、予め存在する微細で反応活性の大きい酸
化チタンが反応の初期におい優先的に一挙に反応して多
量の核を発生させるため、均一かつ微細な粉末が得られ
るものと考えられる。In the present invention, it is not clear how the titanium oxide as an additive contributes to the refinement of the produced titanium carbide, but the pre-existing fine titanium oxide with high reaction activity is preferential at the initial stage of the reaction. It is thought that a uniform and fine powder can be obtained because a large amount of nuclei are generated by reacting all at once.
本発明における焼成温度としては、１３００〜１８００
℃の範囲が好ましく、１３００℃より低いと反応速度が
十分でなく、１８００”Ｃより高いと生成炭化チタンの
異常粒成長により粒子径が大なる傾向を有するとともに
エネルギー的にも経済的でない。また、反応装置内の雰
囲気は反応により生成する一酸化炭素か、またはアルゴ
ンガス等の不活性ガス等により非酸化性ガス雰囲気で行
う必要がある。The firing temperature in the present invention is 1300 to 1800.
℃ range is preferable; if it is lower than 1300''C, the reaction rate is insufficient, and if it is higher than 1800''C, the particle size tends to increase due to abnormal grain growth of the titanium carbide produced, and it is not economical in terms of energy. The atmosphere in the reaction apparatus must be a non-oxidizing gas atmosphere such as carbon monoxide produced by the reaction or an inert gas such as argon gas.
反応圧力は特に限定されず、常圧で十分であるが、反応
速度等を考慮して減圧下で行ってもよい。The reaction pressure is not particularly limited, and normal pressure is sufficient, but the reaction may be carried out under reduced pressure in consideration of the reaction rate and the like.
［実施例］
以下、実施例により本発明をより詳細に説明するが、本
発明は斯かる実施例により限定されるものではない。[Examples] Hereinafter, the present invention will be explained in more detail with reference to Examples, but the present invention is not limited to these Examples.
実施例１〜８
主原料である酸化チタン、炭素粉末よび添加剤として使
用される平均粒径００５μｍ以下の酸化チタンを仕込み
、バインダーとして１５−ｔχのポリビニールアルコー
ルおよび３０ｗｔｚのシ９＄１を含有する水溶液を７０
重量部添加し、湿式混合を行った後、約８畷−径の粒子
になるよう造粒した。Examples 1 to 8 Titanium oxide as the main raw material, carbon powder, and titanium oxide with an average particle size of 005 μm or less used as an additive were prepared, and the binder contained 15-tχ polyvinyl alcohol and 30wtz Si9$1. 70% aqueous solution
After adding part by weight and performing wet mixing, the mixture was granulated into particles with a diameter of about 8 mm.
ついでこの混合物を乾燥した後、黒鉛製の反応容器に入
れ、焼成を行った。得られた粉末は走査型電子顕微鏡に
よりＳＥＭ写真を逼り、５０個の粒子の粒子径を測定し
てその平均を平均粒子径とした、ＳＥＭ写真での観察よ
り、生成した炭化チタンの粒子は異常粒成長した粒子を
含まず、極めて粒径の整った粒子であることがわかった
。After drying this mixture, it was placed in a graphite reaction vessel and fired. The obtained powder was taken through an SEM photograph using a scanning electron microscope, and the particle diameter of 50 particles was measured and the average was taken as the average particle diameter.From the observation with the SEM photograph, the produced titanium carbide particles were It was found that the particles were of extremely uniform size and did not contain particles with abnormal grain growth.
この場合の各原料粉末の組成比、反応条件、生成した炭
化チタンの平均粒径を第１表に示す。Table 1 shows the composition ratio of each raw material powder, reaction conditions, and average particle size of the produced titanium carbide in this case.
比較例１〜３
添加剤として使用される平均粒径０．０５μｍ以下の酸
化チタンを比較例１では０．０３重量部、比較例２．３
では使用しなかったがその他は、実施例と同様の条件で
反応原料を混合し、焼成を行った。Comparative Examples 1 to 3 Titanium oxide with an average particle size of 0.05 μm or less used as an additive was 0.03 parts by weight in Comparative Example 1, and 0.03 parts by weight in Comparative Example 2.3.
The reaction raw materials were mixed and calcined under the same conditions as in the example except that they were not used.
この場合の各原料粉末の組成比、反応条件、生成した炭
化チタンの平均粒径を、同様に第１表に示す。The composition ratio of each raw material powder, reaction conditions, and average particle size of the produced titanium carbide in this case are also shown in Table 1.
［発明の効果コ
本発明の方法によれば、汎用の原料に対し０．０５μｍ
以下の極めて微細な酸化チタンを少量添加することによ
り、焼結性に優れた均一でかつ微細な炭化チタン微粉末
が容易に得られるものである。[Effects of the invention] According to the method of the present invention, 0.05 μm for general-purpose raw materials
By adding a small amount of the following extremely fine titanium oxide, a uniform and fine titanium carbide fine powder with excellent sinterability can be easily obtained.
Claims (1)
〜１８００℃の温度で焼成することにより炭化チタンを
得る方法において、平均粒径０．１〜５μｍの酸化チタ
ン１００重量部に対して、添加剤として平均粒径０．０
５μｍ以下の酸化チタンを０．０５〜３０重量部添加す
ることを特徴とする炭化チタン微粉末の製造方法。(1) Titanium oxide and carbon were heated at 1300°C in a non-oxidizing atmosphere.
In a method for obtaining titanium carbide by firing at a temperature of ~1800°C, an additive having an average particle size of 0.0 to 100 parts by weight of titanium oxide with an average particle size of 0.1 to 5 μm is added.
A method for producing fine titanium carbide powder, which comprises adding 0.05 to 30 parts by weight of titanium oxide having a diameter of 5 μm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1090376A JPH02271919A (en) | 1989-04-10 | 1989-04-10 | Production of fine powder of titanium carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1090376A JPH02271919A (en) | 1989-04-10 | 1989-04-10 | Production of fine powder of titanium carbide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02271919A true JPH02271919A (en) | 1990-11-06 |
Family
ID=13996848
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1090376A Pending JPH02271919A (en) | 1989-04-10 | 1989-04-10 | Production of fine powder of titanium carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02271919A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2078614A1 (en) * | 2008-01-11 | 2009-07-15 | tesa SE | Pigment layer and method for long-term inscription of a substrate with high-energy radiation |
| CN101920958A (en) * | 2010-08-06 | 2010-12-22 | 刘昭晖 | Method for preparing nano zirconium carbide |
| US7939164B2 (en) | 2008-01-11 | 2011-05-10 | Tesa Se | Pigment layer and method of permanently scribing a substrate by means of high-energy radiation |
| US8821991B2 (en) | 2008-01-11 | 2014-09-02 | Tesa Se | Process for preparing titanium carbide |
| US9751769B2 (en) | 2012-06-28 | 2017-09-05 | Nisshin Engineering Inc. | Method for production of titanium carbide nanoparticles |
-
1989
- 1989-04-10 JP JP1090376A patent/JPH02271919A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2078614A1 (en) * | 2008-01-11 | 2009-07-15 | tesa SE | Pigment layer and method for long-term inscription of a substrate with high-energy radiation |
| US7939164B2 (en) | 2008-01-11 | 2011-05-10 | Tesa Se | Pigment layer and method of permanently scribing a substrate by means of high-energy radiation |
| US8821991B2 (en) | 2008-01-11 | 2014-09-02 | Tesa Se | Process for preparing titanium carbide |
| CN101920958A (en) * | 2010-08-06 | 2010-12-22 | 刘昭晖 | Method for preparing nano zirconium carbide |
| US9751769B2 (en) | 2012-06-28 | 2017-09-05 | Nisshin Engineering Inc. | Method for production of titanium carbide nanoparticles |
| KR20190132568A (en) | 2012-06-28 | 2019-11-27 | 닛신 엔지니어링 가부시키가이샤 | Method for production of titanium carbide microparticles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3932594A (en) | Process for the preparation of fine grain metal carbide powders | |
| JPS5850929B2 (en) | Method for manufacturing silicon carbide powder | |
| US4190439A (en) | Process for the preparation of fine grain metal carbide powders and sintered articles therefrom | |
| CN108840681B (en) | Nano boron carbide and preparation method thereof | |
| JPS60221365A (en) | Manufacture of high strength silicon carbide sintered body | |
| JPH0741311A (en) | Production of hexagonal boron nitride powder | |
| JP2021116202A (en) | Hexagonal boron nitride powder, and sintered body raw material composition | |
| JPH02271919A (en) | Production of fine powder of titanium carbide | |
| JPH0362643B2 (en) | ||
| KR100420605B1 (en) | Cabalt Metal Agglomerates, a Process of the Same and Their Use | |
| KR100411998B1 (en) | Cabalt Metal Agglomerates, a Method of Producing Them and Their Use | |
| JPH0323206A (en) | Aluminum nitride powder and its production | |
| JPH0280318A (en) | Synthesis of refractory metal boride having predetermined particle dimension | |
| US3567808A (en) | Production of low density-high strength carbon | |
| JP7356364B2 (en) | Hexagonal boron nitride powder and method for producing hexagonal boron nitride powder | |
| JPS61132509A (en) | Production of silicon carbide | |
| CN108675292A (en) | The method that combination method prepares isotropic graphite material | |
| JP7302123B2 (en) | Fibrous boron carbide and method for producing the same | |
| JP7349921B2 (en) | Hexagonal boron nitride sintered body | |
| JPH02283609A (en) | Production of fine silicon carbide powder | |
| JPS6328873B2 (en) | ||
| JPS63151610A (en) | Raw material composition for producing large-sized carbonaceous material | |
| JPS63123867A (en) | Manufacture of silicon carbide formed body for sintering | |
| JPH01167213A (en) | Production of fine powder of titanium diboride | |
| KR100829230B1 (en) | Preparing method of carbon particle |