JPH05147917A - Production of fine tungsten-based carbide powder - Google Patents
Production of fine tungsten-based carbide powderInfo
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- JPH05147917A JPH05147917A JP3343963A JP34396391A JPH05147917A JP H05147917 A JPH05147917 A JP H05147917A JP 3343963 A JP3343963 A JP 3343963A JP 34396391 A JP34396391 A JP 34396391A JP H05147917 A JPH05147917 A JP H05147917A
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Abstract
Description
【0001】[0001]
【産業上の利用分野】この発明は、切削工具や塑性加工
用耐摩工具などとして広く用いられている各種の炭化タ
ングステン(以下WCで示す)基超硬合金を製造するに
際して、原料粉末として用いるのに適した微細なタング
ステン(W)系炭化物粉末の製造法に関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is used as a raw material powder in the production of various tungsten carbide (hereinafter referred to as WC) based cemented carbides widely used as cutting tools, wear-resistant tools for plastic working, etc. The present invention relates to a method for producing a fine tungsten (W) -based carbide powder suitable for the above.
【0002】[0002]
【従来の技術】従来、WC粉末の製造法として、例えば
特公昭51−29520号公報に記載される方法が知ら
れている。この従来方法は、WO3 粉末に所定量の炭素
粉末を混合し、この混合粉末を、窒素(N2 )またはア
ルゴン(Ar)雰囲気中、1000℃以上の温度で還元
処理し、引続いて、水素(H2 )雰囲気中、1400〜
2000℃の温度で炭化処理すること、によりWC粉末
を製造する方法である。2. Description of the Related Art Conventionally, as a method for producing WC powder, for example, a method described in Japanese Patent Publication No. 51-29520 is known. In this conventional method, WO 3 powder is mixed with a predetermined amount of carbon powder, and the mixed powder is subjected to reduction treatment in a nitrogen (N 2 ) or argon (Ar) atmosphere at a temperature of 1000 ° C. or higher, and subsequently, 1400 in a hydrogen (H 2 ) atmosphere
It is a method of producing a WC powder by carbonizing at a temperature of 2000 ° C.
【0003】[0003]
【発明が解決しようとする課題】一方、近年の切削加工
や塑性加工の省力化および高速化に対する要求は厳し
く、これに伴ない、これに用いられる各種工具を構成す
るWC基超硬合金はより高強度を具備することが要求さ
れるが、上記の従来方法はじめ、その他多くの方法で製
造されたWC粉末は相対的に粗く、通常約1μm以上の
平均粒径をもつものであるため、これを原料粉末として
用いて製造したWC基超硬合金の場合、これらの要求に
十分対応できる高強度を具備しないのが現状である。On the other hand, in recent years, demands for labor saving and speeding up of cutting and plastic working have been strict, and accordingly, WC-based cemented carbide constituting various tools used for this has become more difficult. Although it is required to have high strength, the WC powder produced by the above-mentioned conventional method and many other methods is relatively coarse and usually has an average particle size of about 1 μm or more. In the present situation, WC-based cemented carbide produced by using as a raw material powder does not have high strength that can sufficiently meet these requirements.
【0004】[0004]
【課題を解決するための手段】そこで、本発明者等は、
上述のような観点から、より一段と高強度を有するWC
基超硬合金を製造すべく、これの原料粉末であるWC粉
末に着目し、研究を行なった結果、原料粉末として用い
られるタングステン酸化物(以下、WOxで示す、x:
2〜3)粉末および炭素粉末のほかに、さらにV,C
r,Ta,およびTiの炭化物粉末および酸化物粉末の
うちの1種または2種以上からなる炭・酸化物粉末を用
い、これら原料粉末を、その粒度を、それぞれWOx:
1μm以下、炭素粉末:0.5μm以下、および炭・酸
化物粉末:2μm以下に限定した上で、重量%で(以下
%は重量%を示す)、 炭・酸化物粉末:0.1〜2%、 炭素粉末:12〜30%、 WOx粉末:残り、 の配合組成に配合し、混合した後、この混合粉末に、H
2 と、N2 およびArのいずれか、または両方との混合
雰囲気中、望ましくは前半を相対的にN2 および/また
はArの割合を多くし、後半を相対的にH2 の割合を多
くしたH2 と、N2 および/またはArとの混合雰囲気
中、1000〜1600℃の温度で還元炭化処理を施す
と、平均粒径で0.5μm以下の微細なW系炭化物粉末
が製造でき、かつこのW系炭化物粉末を用いて製造した
WC基超硬合金は一段と高強度をもつようになるという
研究結果を得たのである。Therefore, the present inventors have
From the above viewpoints, WC having much higher strength
In order to produce a base cemented carbide, attention has been paid to WC powder, which is a raw material powder of the base cemented carbide, and as a result of research, a tungsten oxide (hereinafter referred to as WOx, x:
2-3) In addition to powder and carbon powder, V, C
A carbon / oxide powder composed of one or more of carbide powders and oxide powders of r, Ta, and Ti was used, and these raw material powders had particle sizes of WOx:
1 μm or less, carbon powder: 0.5 μm or less, and carbon / oxide powder: 2 μm or less, and in% by weight (hereinafter,% means% by weight), carbon / oxide powder: 0.1 to 2 %, Carbon powder: 12 to 30%, WOx powder: rest, and after blending in a blending composition of
In a mixed atmosphere of 2, and one or both of N 2 and Ar, preferably, the proportion of N 2 and / or Ar was relatively increased in the first half, and the proportion of H 2 was relatively increased in the latter half. When a reducing carbonization treatment is performed at a temperature of 1000 to 1600 ° C. in a mixed atmosphere of H 2 and N 2 and / or Ar, a fine W-based carbide powder having an average particle size of 0.5 μm or less can be produced, and The research result was obtained that the WC-based cemented carbide produced by using this W-based carbide powder has higher strength.
【0005】この発明は、上記の研究結果にもとづいて
なされたものであって、 (a) 原料粉末として、平均粒径:1μm以下のWO
x粉末、同0.5μm以下の炭素粉末、並びに同2μm
以下のV,Cr,Ta、およびTiの炭化物粉末および
酸化物粉末のうちの1種または2種以上からなる炭・酸
化物粉末を用い、 (b) これら原料粉末を、重量%で(以下%は重量%
を示す)、 炭・酸化物粉末:0.1〜2%、 炭素粉末:12〜30%、 WOx粉末:残り、 の配合組成に配合し、混合した後、 (c) この混合粉末に、H2 +N2 および/またはA
rの混合雰囲気中、1000〜1600℃の温度で還元
炭化処理を施すこと、 により平均粒径で0.5μm以下の微細なW系炭化物粉
末を製造する方法に特徴を有するものである。The present invention has been made based on the above research results. (A) As a raw material powder, WO having an average particle size of 1 μm or less is used.
x powder, carbon powder of 0.5 μm or less, and 2 μm
Using carbon / oxide powders consisting of one or more of the following V, Cr, Ta, and Ti carbide powders and oxide powders, (b) these raw material powders in weight% (hereinafter% Is% by weight
Of the following formulas), carbon / oxide powder: 0.1 to 2%, carbon powder: 12 to 30%, WOx powder: the rest, and then mixed (C) 2 + N 2 and / or A
It is characterized by a method for producing a fine W-based carbide powder having an average particle size of 0.5 μm or less by performing a reducing carbonization treatment at a temperature of 1000 to 1600 ° C. in a mixed atmosphere of r.
【0006】つぎに、この発明の方法において、製造条
件を上記の通りに限定した理由を説明する。 A. 原料粉末の平均粒径 (a) WOx粉末 その平均粒径が1μmを越えると、他の原料粉末との均
一混合が困難となり、この結果還元炭化反応が不均一と
なるばかりでなく、部分的粒成長が起って平均粒径で
0.5μm以下のW系炭化物粉末を製造することができ
なくなることから、その平均粒径を1μm以下と定め
た。Next, the reason why the manufacturing conditions are limited as described above in the method of the present invention will be explained. A. Average particle size of raw material powder (a) WOx powder When the average particle size exceeds 1 μm, uniform mixing with other raw material powder becomes difficult, resulting in non-uniform reduction carbonization reaction and partial particle size Since W-based carbide powder having an average particle size of 0.5 μm or less cannot be produced due to the growth, the average particle size is defined as 1 μm or less.
【0007】(b) 炭・酸化物粉末および炭素粉末 これら原料粉末の平均粒径が、それぞれ2μmおよび
0.5μmを越えると、それぞれのもつ作用、すなわち
粒成長抑制作用、並びに還元炭化作用が局部的になっ
て、微細にして整粒のW系炭化物粉末の製造が困難にな
ることから、その平均粒径をそれぞれ2μm以下および
0.5μm以下と定めた。(B) Carbon / oxide powder and carbon powder When the average particle size of these raw material powders exceeds 2 μm and 0.5 μm, respectively, their respective functions, that is, the grain growth suppressing effect and the reducing carbonizing effect are locally present. Since it becomes difficult to produce finely sized W-based carbide powder, the average particle diameters thereof are set to 2 μm or less and 0.5 μm or less, respectively.
【0008】B. 原料粉末の配合組成 (a) 炭・酸化物粉末 これらの粉末には、還元炭化処理過程での粒成長を抑制
し、もって製造されたW系炭化物粉末を平均粒径で0.
5μm以下に微細化する作用があるが、その割合が0.
1%未満では前記作用に所望の効果が得られず、一方そ
の割合が2%を越えると、WC基超硬合金の製造時に複
炭化物として析出し、強度を低下させることから、その
割合を0.1〜2%と定めた。B. Composition of Raw Material Powder (a) Carbon / Oxide Powder These powders suppress the grain growth in the reduction carbonization process, and the W-based carbide powder thus produced has an average particle size of 0.
There is an effect of making the particles finer than 5 μm, but the ratio is 0.
If it is less than 1%, the desired effect cannot be obtained, while if it exceeds 2%, it precipitates as a double carbide during the production of a WC-based cemented carbide, which lowers the strength. It was set to 1 to 2%.
【0009】(b) 炭素粉末 その割合が12%未満では、炭素不足が原因で、炭化処
理後の粉末中に、WやV、さらにM2 C型炭化物などが
混入するようになり、一方その割合が30%を越える
と、炭素過剰が原因で遊離炭素が残存するようになるこ
とから、その割合を12〜30%と定めた。(B) Carbon powder If the ratio is less than 12%, W and V, and further M 2 C type carbides will be mixed in the powder after carbonization due to carbon deficiency. If the ratio exceeds 30%, free carbon will remain due to excess carbon, so the ratio was defined as 12 to 30%.
【0010】C. 還元炭化処理温度 その温度が1000℃未満では、還元炭化反応の進行が
遅く、この結果製造される粉末中に金属やM2 C型炭化
物などが混入するようになり、一方その温度が1600
℃を越えると粒成長が起って、平均粒径で0.5μm以
下の微細粉末を製造することができなくなることから、
その温度を1000〜1600℃と定めた。C. Reducing carbonization temperature If the temperature is less than 1000 ° C., the reducing carbonization reaction proceeds slowly, and as a result, metal or M 2 C type carbide is mixed in the produced powder, while the temperature is 1600.
If the temperature exceeds ℃, grain growth occurs and it becomes impossible to produce a fine powder having an average grain size of 0.5 μm or less.
The temperature was set to 1000 to 1600 ° C.
【0011】[0011]
【実施例】つぎに、この発明の方法を実施例により具体
的に説明する。それぞれ表1に示される平均粒径をもっ
た原料粉末を用い、これら原料粉末を同じく表1に示さ
れる配合組成に配合し、ボールミルにて72時間湿式混
合し、乾燥した後、表2に示される条件で還元炭化処理
を行なうことにより本発明法1〜8および従来法1〜3
を実施し、それぞれ表2に示される平均粒径をもったW
系炭化物粉末およびWC粉末を製造した。EXAMPLES Next, the method of the present invention will be specifically described by way of Examples. Raw material powders each having the average particle size shown in Table 1 were used, and these raw material powders were similarly compounded to the compounding composition shown in Table 1, wet-mixed for 72 hours in a ball mill, dried, and then shown in Table 2. The present invention methods 1 to 8 and conventional methods 1 to 3 are carried out by reducing carbonization treatment under the following conditions.
And W having the average particle size shown in Table 2 respectively.
A system carbide powder and a WC powder were produced.
【0012】[0012]
【表1】 [Table 1]
【0013】[0013]
【表2】 [Table 2]
【0014】ついで、この結果得られた各種の粉末に、
平均粒径:1.2μmのCo粉末をいずれも10%配合
し、ボールミルにて72時間湿式混合し、乾燥した後、
1ton /cm2 の圧力が圧粉体にプレス成形し、この圧粉
体を真空雰囲気中、温度:1380℃に2時間保持の条
件で焼結してWC基超硬合金を製造し、このWC基超硬
合金の抗析力を測定し、強度を評価した。この測定結果
を表2に示した。Then, various powders obtained as a result are
10% of each Co powder having an average particle diameter of 1.2 μm was blended, wet-mixed in a ball mill for 72 hours, dried, and then
A WC-based cemented carbide is manufactured by press-forming a green compact with a pressure of 1 ton / cm 2 and sintering the green compact in a vacuum atmosphere at a temperature of 1380 ° C. for 2 hours. The segregation force of the base cemented carbide was measured to evaluate the strength. The measurement results are shown in Table 2.
【0015】[0015]
【発明の効果】表1,2に示される結果から、本発明法
1〜8によれば、従来法1〜3により製造されたWC粉
末に比して、一段と微細なW系炭化物粉末を製造するこ
とができ、したがってこれを用いて製造したWC基超硬
合金は従来法1〜3により製造されたWC粉末を用いて
製造した場合に比して、きわめて高い強度をもつように
なるのである。From the results shown in Tables 1 and 2, according to the methods 1 to 8 of the present invention, a finer W-based carbide powder is produced as compared with the WC powders produced by the conventional methods 1 to 3. Therefore, the WC-based cemented carbide produced using this has extremely high strength as compared with the case where the WC powder produced by the conventional methods 1 to 3 is used. ..
【0016】上述のように、この発明の方法によれば、
平均粒径で0.5μm以下のきわめて微細なW系炭化物
粉末を製造することができ、かつこれを用いて製造した
WC基超硬合金は、高強度を具備するようになるので、
高強度が要求される各種の切削加工や塑性加工分野です
ぐれた性能を発揮するようになるなど工業上有用な効果
がもたらされるのである。As mentioned above, according to the method of the present invention,
Since an extremely fine W-based carbide powder having an average particle size of 0.5 μm or less can be produced, and a WC-based cemented carbide produced by using the same has high strength,
Industrially useful effects such as excellent performance in various cutting and plastic working fields that require high strength are brought about.
【手続補正書】[Procedure amendment]
【提出日】平成4年2月20日[Submission date] February 20, 1992
【手続補正1】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】0009[Correction target item name] 0009
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【0009】 (b) 炭素粉末 その割合が12%未満では、炭素不足が原因で、炭化処
理後の粉末中に、WやVなどの金属成分、さらにM2 C
型炭化物などが混入するようになり、一方その割合が3
0%を越えると、炭素過剰が原因で遊離炭素が残存する
ようになることから、その割合を12〜30%と定め
た。(B) Carbon powder If the ratio is less than 12%, due to carbon deficiency, in the powder after carbonization treatment , metal components such as W and V, and further M 2 C are added.
Type carbides are mixed in, while the ratio is 3
If it exceeds 0%, free carbon will remain due to excess carbon, so the ratio was set to 12 to 30%.
【手続補正2】[Procedure Amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】0014[Correction target item name] 0014
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【0014】 ついで、この結果得られた各種の粉末
に、平均粒径:1.2μmのCo粉末をいずれも10%
配合し、ボールミルにて72時間湿式混合し、乾燥した
後、1ton /cm2 の圧力で圧粉体にプレス成形し、この
圧粉体を真空雰囲気中、温度:1380℃に2時間保持
の条件で焼結してWC基超硬合金を製造し、このWC基
超硬合金の抗析力を測定し、強度を評価した。この測定
結果を表2に示した。Next, 10% of Co powder having an average particle diameter of 1.2 μm was added to each of the various powders obtained as a result.
Blending, wet mixing in a ball mill for 72 hours, drying, and press molding into a green compact at a pressure of 1 ton / cm 2 , and the green compact is held in a vacuum atmosphere at a temperature of 1380 ° C. for 2 hours. Was sintered to manufacture a WC-based cemented carbide, and the anti-segregation force of this WC-based cemented carbide was measured to evaluate the strength. The measurement results are shown in Table 2.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 篠原 耕治 埼玉県大宮市北袋町1−297 三菱マテリ アル株式会社中央研究所内 (72)発明者 植田 文洋 埼玉県大宮市北袋町1−297 三菱マテリ アル株式会社中央研究所内 (72)発明者 棚瀬 照義 岐阜県安八郡神戸町大字横井字中新田1528 三菱マテリアル株式会社岐阜製作所内 (72)発明者 小林 勝己 埼玉県大宮市北袋町1−297 三菱マテリ アル株式会社中央研究所内 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Koji Shinohara 1-297 Kitabukuro-cho, Omiya-shi, Saitama Prefecture Central Research Laboratory, Mitsubishi Materialial Co., Ltd. (72) Fumihiro Ueda 1-297 Kitabukuro-cho, Omiya-shi, Saitama Mitsubishi Materials Central Research Institute Co., Ltd. (72) Teruyoshi Tanase, Inventor Teruyoshi Tanase, Kobe, Anpachi-gun, Gifu Prefecture Nakai, Nakata 1528 Mitsubishi Materials Corporation Gifu Manufacturing Co., Ltd. (72) Inventor Katsumi Kobayashi 1-297 Kitabukuro, Omiya, Saitama Mitsubishi Materi Al Central Research Institute
Claims (2)
のタングステン酸化物粉末、同0.5μm以下の炭素粉
末、並びに同2μm以下のV,Cr,Ta、およびTi
の炭化物粉末および酸化物粉末のうちの1種または2種
以上からなる炭・酸化物粉末を用い、 これら原料粉末を、重量%で、 炭・酸化物粉末:0.1〜2%、 炭素粉末:12〜30%、 タングステン酸化物粉末:残り、 の配合組成に配合し、混合した後、 この混合粉末に、水素と、窒素およびアルゴンのいずれ
か、または両方との混合雰囲気中、1000〜1600
℃の温度で還元炭化処理を施すこと、を特徴とする平均
粒径で0.5μm以下の微細なタングステン系炭化物粉
末の製造法。1. As raw material powders, a tungsten oxide powder having an average particle diameter of 1 μm or less, a carbon powder having an average particle diameter of 0.5 μm or less, and V, Cr, Ta, and Ti having an average particle diameter of 2 μm or less.
Of one or two or more of the above-mentioned carbide powder and oxide powder are used, and these raw material powders are represented by% by weight: carbon / oxide powder: 0.1 to 2%, carbon powder 12 to 30%, Tungsten oxide powder: the rest, after blending and mixing in a blending composition of 1000 to 1600 in this mixed powder in a mixed atmosphere of hydrogen and either or both of nitrogen and argon.
A method for producing a fine tungsten-based carbide powder having an average particle size of 0.5 μm or less, which is characterized in that a reducing carbonization treatment is performed at a temperature of ° C.
的に窒素およびアルゴンのいずれか、または両方の割合
を多くし、同後半の雰囲気を相対的に水素の割合を多く
した水素と、窒素およびアルゴンのいずれか、または両
方との混合雰囲気としたことを特徴とする上記請求項1
記載の微細なタングステン系炭化物粉末の製造法。2. The atmosphere in the first half of the reduction carbonization treatment is relatively enriched with nitrogen and / or argon, and the atmosphere in the latter half is relatively enriched with hydrogen and nitrogen. 2. A mixed atmosphere of either or both of argon and argon, or both of them.
A method for producing the fine tungsten-based carbide powder described.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3343963A JPH05147917A (en) | 1991-12-02 | 1991-12-02 | Production of fine tungsten-based carbide powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3343963A JPH05147917A (en) | 1991-12-02 | 1991-12-02 | Production of fine tungsten-based carbide powder |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH05147917A true JPH05147917A (en) | 1993-06-15 |
Family
ID=18365595
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP3343963A Withdrawn JPH05147917A (en) | 1991-12-02 | 1991-12-02 | Production of fine tungsten-based carbide powder |
Country Status (1)
Country | Link |
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JP (1) | JPH05147917A (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0697465A1 (en) * | 1994-08-15 | 1996-02-21 | Iscar Ltd. | Tungsten-based cemented carbide powder mix and cemented carbide products made therefrom |
EP0808912A1 (en) * | 1996-05-21 | 1997-11-26 | Tokyo Tungsten Co., Ltd. | Composite carbide powder used for cemented carbide and method of producing the same |
CN107867691A (en) * | 2017-11-30 | 2018-04-03 | 株洲三鑫硬质合金生产有限公司 | A kind of preparation method and application of high-quality coarse-grained WC powder |
WO2020230543A1 (en) | 2019-05-13 | 2020-11-19 | 住友電気工業株式会社 | Tungsten carbide powder and production method therefor |
-
1991
- 1991-12-02 JP JP3343963A patent/JPH05147917A/en not_active Withdrawn
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0697465A1 (en) * | 1994-08-15 | 1996-02-21 | Iscar Ltd. | Tungsten-based cemented carbide powder mix and cemented carbide products made therefrom |
EP0808912A1 (en) * | 1996-05-21 | 1997-11-26 | Tokyo Tungsten Co., Ltd. | Composite carbide powder used for cemented carbide and method of producing the same |
CN107867691A (en) * | 2017-11-30 | 2018-04-03 | 株洲三鑫硬质合金生产有限公司 | A kind of preparation method and application of high-quality coarse-grained WC powder |
CN107867691B (en) * | 2017-11-30 | 2020-07-31 | 株洲三鑫硬质合金生产有限公司 | Preparation method and application of high-quality coarse grain WC powder |
WO2020230543A1 (en) | 2019-05-13 | 2020-11-19 | 住友電気工業株式会社 | Tungsten carbide powder and production method therefor |
KR20220007062A (en) | 2019-05-13 | 2022-01-18 | 스미토모덴키고교가부시키가이샤 | Tungsten carbide powder and its manufacturing method |
US11396451B2 (en) | 2019-05-13 | 2022-07-26 | Sumitomo Electric Industries, Ltd. | Tungsten carbide powder and production method therefor |
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