JPS61132511A - Production of tib2 powder - Google Patents
Production of tib2 powderInfo
- Publication number
- JPS61132511A JPS61132511A JP25133684A JP25133684A JPS61132511A JP S61132511 A JPS61132511 A JP S61132511A JP 25133684 A JP25133684 A JP 25133684A JP 25133684 A JP25133684 A JP 25133684A JP S61132511 A JPS61132511 A JP S61132511A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- tib2
- weight ratio
- particle size
- 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
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は均一かつ嶺細なＴｉＢ２粉末の製造方法に関す
るものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing uniform and fine TiB2 powder.
ＴｉＢ２は高融点、高硬度を持ち、耐熱性、耐摩耗性等
に優れることがら超硬耐熱材料として注目されており、
切削工具材料、ロケット材料、熱機関部品等に利用され
ている。しかしこのような特長を有するＴｉＢ２は難焼
結性物質であり１通常はホットプレス法によって焼結体
を得ており。TiB2 has a high melting point, high hardness, and is attracting attention as a carbide heat-resistant material because of its excellent heat resistance and wear resistance.
It is used for cutting tool materials, rocket materials, heat engine parts, etc. However, TiB2, which has such characteristics, is a material that is difficult to sinter, and sintered bodies are usually obtained by hot pressing.
特にその原料粉末として均一かつ微細なＴｉＢ２が要求
されている。In particular, uniform and fine TiB2 is required as the raw material powder.
ＴｉＢ２粉末を工業的ミ製造する方法には。A method for industrially producing TiB2 powder.
公知なものとしてＴ ｉ Ｏ２をＣによってアルゴン等
の不活性ガス雰囲気中にて１４００℃以上で還元すると
同時に８２０３を用いて少なくとも１６００℃以上で硼
化する方法が挙げられる。A known method includes reducing T i O2 with C at 1400° C. or higher in an atmosphere of an inert gas such as argon, and at the same time borating using 8203 at at least 1600° C. or higher.
しかしこの方法によって得られたＴｉＢ２粉末の粒径は
、熱処理温度が高いために粒成長が避けられず、一般に
は、２〜２０＃Ｌｍ程度になり、そのほとんどが５１Ｌ
ｍ以上である。しかも粒度分布の巾も大きくなる。また
未反応のＣが遊離炭素としてかなり残留しているという
欠点がある。However, the particle size of the TiB2 powder obtained by this method is generally about 2 to 20 #Lm, and most of them are about 51Lm because grain growth is unavoidable due to the high heat treatment temperature.
m or more. Furthermore, the width of the particle size distribution also increases. Another drawback is that a considerable amount of unreacted C remains as free carbon.
本発明は以上の欠点を解決することを目的としたもので
あり１粒径が均一でかつ２ｐｍ以下のＴｉＢ２粉末を製
造する方法を提供するものである。The present invention aims to solve the above-mentioned drawbacks and provides a method for producing TiB2 powder having a uniform grain size of 2 pm or less.
Ｔ ｉ Ｏ２をＣで還元し、さらにＢ２０３で硼化して
ＴｉＢ２を得る反応は次式のように表わされる。The reaction of reducing T i O2 with C and further boronizing with B203 to obtain TiB2 is expressed by the following formula.
Ｔ ｉ ０２ ＋Ｂ２０３ ＋５Ｃ
＃ ＴｉＢ２＋５ＣＯ
ここで化学量論的にはＴｉＯ２：１に対してＢ２０３
： ０．８７ （重量比）およびＣ：０．７５（重量
比〕が必要であるが、該反応に８いて、Ｂ２Ｏ３は高温
下での蒸気圧が高いために揮発損失しやすいことから過
剰に添加しなければならない。ざらにＣについても未反
応Ｔ ｉ Ｏ２の残留をなくすために過剰量が必要であ
る。T i 02 +B203 +5C # TiB2+5CO Here, stoichiometrically, B203 for TiO2:1
: 0.87 (weight ratio) and C: 0.75 (weight ratio). An excess amount of C is also required to eliminate the residual unreacted T i O2.
そこで本発明者等の実験によれば、出発原料としてＴ
ｉ Ｏ２粉末１に対してＢ２０３粉末を１．１３〜２．
１８（重量比）、炭素質物質０．８０〜１．１３（重量
比）を均一になるように混合する。According to the experiments conducted by the present inventors, T.
i O2 powder to 1:1.13-2.
18 (weight ratio) and carbonaceous material 0.80 to 1.13 (weight ratio) are mixed uniformly.
そしてこの混合物を保形性が可能な程度に、圧縮成型し
、５０ Ｔｏｒｒ以下、より好ましくは２０Ｔ ａｒｒ
以下の減圧下にて１３００−１６００°Ｃの温度まで昇
温加熱した結果、粒径が０．５〜２４ｍ程度の微細なＴ
ｉＢ２粉末を得ることができることが判明した。Then, this mixture is compression molded to the extent that shape retention is possible, and the temperature is 50 Torr or less, more preferably 20 Torr or less.
As a result of heating to a temperature of 1300-1600°C under the following reduced pressure, fine T with a particle size of about 0.5 to 24 m was produced.
It has been found that iB2 powder can be obtained.
原料粉末の組成比および製造条件を限定した理由につい
ては以下に詳細に説明する。The reason for limiting the composition ratio of the raw material powder and the manufacturing conditions will be explained in detail below.
まず８２０３ Ｍについては、Ｔ ｉ Ｏ２粉末ｌに対
して１．１３〜２． Ｊ、 ８ （重量比）が好ましく
、これは化学量論組成の１．３〜２．５倍量に相当する
。First, for 8203 M, the ratio is 1.13 to 2. J, 8 (weight ratio) is preferred, which corresponds to 1.3 to 2.5 times the stoichiometric composition.
しかし１．１３（重量比）以下になると、加熱時のＢ２
Ｏ３の揮発損失にもとづくＢ源の不足となり、反応生成
物がＴｉＢ２の他にＴｉＣの２相となり、好ましくない
。一方２．１８（重量比）以上になると１反応生成物は
Ｔ ｔ Ｂ ２単−相になるが、反応に関与しないＢ２
Ｏ３が多くなり経済性の面で適切でない。However, if it becomes less than 1.13 (weight ratio), B2 during heating
The B source becomes insufficient due to the volatilization loss of O3, and the reaction product becomes two phases of TiC in addition to TiB2, which is not preferable. On the other hand, when the weight ratio exceeds 2.18, 1 reaction product becomes a T t B 2 single phase, but B2 that does not participate in the reaction
The amount of O3 increases, making it unsuitable from an economic point of view.
次にＣ量については０．８０−１．１３（重量比）の範
囲が好ましく、Ｏ，ａＯ（重量比）以下では、Ｃ源の不
足にもとづく未反応のＴ ｉ Ｏ２が残留しやすくなり
、１．１３（重量比）以上では遊ｇＩ炭素としてＴｉＢ
２粉末中に残留するために純度的に好ましくない。Next, the amount of C is preferably in the range of 0.80-1.13 (weight ratio), and if it is less than O, aO (weight ratio), unreacted TiO2 tends to remain due to lack of C source, At 1.13 (weight ratio) or more, TiB is used as free gI carbon.
2. Since it remains in the powder, it is unfavorable in terms of purity.
次に製造条件について粉末製造用炉内圧が５０Ｔ ｏｒ
ｒ以上になると、１３００〜１６００℃の温度範囲では
、該反応が十分に進行せずこれを促進するには、加熱温
度を高める必要があり、これは生成したＴｉＢ２の粒成
長を促がし本発明の目的である均一、かつ微細なＴ ｉ
Ｂ ２粉末を得ることが困難となる。Next, regarding the manufacturing conditions, the pressure inside the furnace for powder manufacturing is 50T or
When the temperature exceeds r, the reaction does not proceed sufficiently in the temperature range of 1300 to 1600°C, and it is necessary to increase the heating temperature to promote it. Uniform and fine Ti which is the object of the invention
It becomes difficult to obtain B2 powder.
また加熱温度について１３００℃以下では、該反応が進
まないか、または１反応時間が非常に長くなる。さらに
、１６００℃以上では粒成長が避けられないので好まし
くない。Further, if the heating temperature is 1300° C. or lower, the reaction will not proceed or one reaction time will be extremely long. Further, if the temperature is 1600° C. or higher, grain growth is unavoidable, which is not preferable.
以上の条件によって得られたＴ ｉ Ｂ ２粉末は従来
の方法によるものに比べて均一で、微細な粒径を有する
ものである。The T i B 2 powder obtained under the above conditions is more uniform and has a finer particle size than that obtained by the conventional method.
実施例１
平均粒径０．１．ｇ、ｍのＴ ｉＯ２粉末１に対して平
均粒径ＬＯｐｍのＢ２０３粉末１．３１（重量比）およ
び平均粒径２０ｍｐｍの炭素粉末０．８３（重量比）を
アルミナ製ボールミルによって混合し、この混合物をタ
ブレット状（約１５ｍｍφ×１０ｍｍＨ）に成型後、タ
フ −７７炉で０．３Ｔｏｒｒ、１４００℃、１時間の
条件で加熱処理した。得られたＴｉＢ２粉末は残留Ｃが
０．２％で、粒径０．５〜１沖ｍの微細な粉末であった
。Example 1 Average particle size 0.1. B203 powder with an average particle size of LOpm 1.31 (weight ratio) and carbon powder with an average particle size of 20 mpm 0.83 (weight ratio) were mixed with 1 g, m of TiO2 powder using an alumina ball mill, and this mixture After molding into a tablet shape (approximately 15 mmφ x 10 mmH), it was heat-treated in a Tough-77 furnace at 0.3 Torr and 1400° C. for 1 hour. The obtained TiB2 powder had a residual C content of 0.2% and was a fine powder with a particle size of 0.5 to 1 mm.
実施例２
実施例１と同様の方法で得た混合物の成型体をタンマン
炉で１Ｔｏｒｒ、１５００℃、１時間の条件で加熱処理
した。得られたＴｉＢ２粉末は残留Ｃが０．３％で粒径
０．５〜１１−５ｐの微細な粉末であった。Example 2 A molded body of the mixture obtained in the same manner as in Example 1 was heat-treated in a Tammann furnace at 1 Torr, 1500° C., and for 1 hour. The obtained TiB2 powder was a fine powder with a residual C content of 0.3% and a particle size of 0.5 to 11-5p.
比較例
実施例１と同様の方法で得た混合物の成型体を、タンマ
ン炉でアルゴンガス気流中において。Comparative Example A molded body of the mixture obtained in the same manner as in Example 1 was placed in a Tammann furnace in an argon gas stream.
１７００’ｃ！、１時間の条件で加熱処理して得られた
Ｔ ｉ Ｂ ２粉末は、残留Ｃが０．４％で粒径が２〜
８ｐｍであり１本発明による方法に比べると大きいもの
であった。1700'c! The T i B 2 powder obtained by heat treatment under the conditions of , 1 hour has a residual C of 0.4% and a particle size of 2 to
8 pm, which was larger than the method according to the present invention.
本発明方法により従来の２〜２０ｇｍのＴｉＢ２に比し
、均一で２ルｍ以下の微細なＴ ｉ Ｂ ２の粉末を製
造することが粧能となり、超硬耐熱材料等先進分野のす
ぐれた材料を容易に得ることかできる効果を奏する。By the method of the present invention, compared to the conventional TiB2 of 2 to 20 gm, it is possible to produce uniform and fine TiB2 powder of 2 μm or less, and it can be used as an excellent material in advanced fields such as carbide heat-resistant materials. This has the effect of making it easy to obtain.
Claims (1)
１３〜２．１８（重量比）、炭素質物質を０．８０〜１
．１３（重量比）混合し、５０Ｔｏｒｒ以下の減圧下に
て１３００〜１６００℃の範囲内で加熱することを特徴
とするＴｉＢ＿２粉末の製造方法。1 B_2O_3 powder for 1 part of TiO_2 powder.
13-2.18 (weight ratio), carbonaceous material 0.80-1
．． A method for producing TiB_2 powder, which is characterized by mixing 13 (weight ratio) and heating within a range of 1300 to 1600°C under reduced pressure of 50 Torr or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25133684A JPS61132511A (en) | 1984-11-28 | 1984-11-28 | Production of tib2 powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25133684A JPS61132511A (en) | 1984-11-28 | 1984-11-28 | Production of tib2 powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61132511A true JPS61132511A (en) | 1986-06-20 |
Family
ID=17221307
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25133684A Pending JPS61132511A (en) | 1984-11-28 | 1984-11-28 | Production of tib2 powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61132511A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0503930A2 (en) * | 1991-03-13 | 1992-09-16 | Advanced Ceramics Corporation | Production of titanium diboride and boron nitride powders |
| WO2013023460A1 (en) * | 2012-03-07 | 2013-02-21 | 深圳市新星轻合金材料股份有限公司 | Cycled preparation method that uses mixture of sodium-based titanium and boron fluoride salts as intermediate raw material and produces titanium boride and simultaneously sodium cryolite |
| EP2636645A1 (en) * | 2012-03-07 | 2013-09-11 | Shenzhen Sunxing Light Alloys Materials Co., Ltd | Cyclic preparation method for producing titanium boride from intermediate feedstock potassium-based titanium-boron-fluorine salt mixture and producing potassium cryolite as byproduct |
-
1984
- 1984-11-28 JP JP25133684A patent/JPS61132511A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0503930A2 (en) * | 1991-03-13 | 1992-09-16 | Advanced Ceramics Corporation | Production of titanium diboride and boron nitride powders |
| WO2013023460A1 (en) * | 2012-03-07 | 2013-02-21 | 深圳市新星轻合金材料股份有限公司 | Cycled preparation method that uses mixture of sodium-based titanium and boron fluoride salts as intermediate raw material and produces titanium boride and simultaneously sodium cryolite |
| EP2636644A1 (en) * | 2012-03-07 | 2013-09-11 | Shenzhen Sunxing Light Alloys Materials Co., Ltd | Cyclic preparation method for producing titanium boride from intermediate feedstock sodium-based titanium-boron-fluorine salt mixture and producing sodium cryolite as byproduct |
| EP2636645A1 (en) * | 2012-03-07 | 2013-09-11 | Shenzhen Sunxing Light Alloys Materials Co., Ltd | Cyclic preparation method for producing titanium boride from intermediate feedstock potassium-based titanium-boron-fluorine salt mixture and producing potassium cryolite as byproduct |
| GB2510008A (en) * | 2012-03-07 | 2014-07-23 | Shenzhen Sunxing Light Alloys Materials Co Ltd | Cycled preparation method that uses mixture of sodium-based titanium and boron fluoride salts as intermediate raw material and produces titanium boride |
| GB2510008B (en) * | 2012-03-07 | 2015-09-09 | Shenzhen Sunxing Light Alloys Materials Co Ltd | Cyclic preparation method for producing titanium boride from intermediate feedstock Na-based Ti-B-F salt mixture and producing sodium cryolite as byproduct |
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