JPS61201708A - Manufacture of molybdenum powder - Google Patents
Manufacture of molybdenum powderInfo
- Publication number
- JPS61201708A JPS61201708A JP4151885A JP4151885A JPS61201708A JP S61201708 A JPS61201708 A JP S61201708A JP 4151885 A JP4151885 A JP 4151885A JP 4151885 A JP4151885 A JP 4151885A JP S61201708 A JPS61201708 A JP S61201708A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- molybdenum
- reduction
- molybdenum oxide
- temp
- 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
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000000843 powder Substances 0.000 claims abstract description 29
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 14
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 13
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 26
- 230000005484 gravity Effects 0.000 abstract description 11
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 abstract description 7
- 238000005245 sintering Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000010419 fine particle Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012190 activator Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、粉末冶金法において使用されるモリブデン粉
末の製法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for producing molybdenum powder used in powder metallurgy.
（従来の技術）
粉末冶金法の原料となる金属モリブデン粉末は、酸化モ
リブデン粉末を比較的低温の一次還元と比較的高温の二
次還元の２回に分けて水素還元して製造する（２段還元
法）のが一般的である。(Prior art) Metallic molybdenum powder, which is a raw material for powder metallurgy, is produced by reducing molybdenum oxide powder with hydrogen in two stages: primary reduction at a relatively low temperature and secondary reduction at a relatively high temperature. (reduction method) is common.
このような一般的な方法とは別に、例えば三酸化モリブ
デン粉末（Ｍ ｏ ０３）を水素雰囲気炉中で最高１１
００℃以上の温度まで時間をかけて徐々に昇温し加熱す
ることによって１段で金属粉末に還元する方法（１段還
元法）もある。Apart from these common methods, for example, molybdenum trioxide powder (M o 03) can be heated up to 11% in a hydrogen atmosphere furnace.
There is also a method (one-stage reduction method) in which metal powder is reduced in one step by gradually raising the temperature to a temperature of 00° C. or higher over time.
（発明が解決しようとする問題点）
上記従来の製法のうち、２段還元法は、還元を２回に分
けて行なわなければならないので、それだけ手間がかか
り、必要な装置も多くなるという問題点があった。また
上記従来の１段還元法は。(Problems to be Solved by the Invention) Among the conventional production methods mentioned above, the two-stage reduction method requires reduction to be carried out in two steps, which is time-consuming and requires more equipment. was there. Also, the conventional one-stage reduction method mentioned above.
２段還元法に較べて工程が簡単であるという利点はある
が、得られる金属粉末の粒度が粗く、圧粉体を焼結した
ときに充分な比重が得られないという問題があり、通常
のモリブデンワイヤ等の工業生産に採用することができ
なかった。Although it has the advantage that the process is simpler than the two-stage reduction method, there is a problem that the particle size of the obtained metal powder is coarse and sufficient specific gravity cannot be obtained when the green compact is sintered. It could not be adopted for industrial production of molybdenum wire, etc.
（問題点を解決するための手段） 本発明は、上記従来の製法の問題点を解決し。(Means for solving problems) The present invention solves the problems of the conventional manufacturing method described above.
粒度が細かく焼結時に高比重の得られる粉末を得るため
１次のような構成とした。In order to obtain a powder with fine particle size and high specific gravity upon sintering, the following structure was adopted.
すなわち、本発明にかかるモリブデン粉末の製法は、０
．００２５〜０．０３重量％のニッケルを添加した酸化
モリブデン粉末を水素雰囲気中で低温から徐々に１００
０℃以上の高温に加熱し、酸化モリブデン粉末を還元し
て微量のニッケルを含有する金属モリブデン粉末を得る
ことを特徴としている。That is, the method for producing molybdenum powder according to the present invention has 0
．． Molybdenum oxide powder to which 0.025 to 0.03% by weight of nickel has been added is gradually heated to 100% by weight from a low temperature in a hydrogen atmosphere.
It is characterized by heating to a high temperature of 0° C. or higher to reduce molybdenum oxide powder to obtain metal molybdenum powder containing a trace amount of nickel.
これについて具体的に例を挙げて説明すれば、以下の通
りである。A specific example of this will be explained below.
先ず原料である酸化モリブデン（Ｍ ｏ Ｏｘ、通常は
三酸化モリブデンＭ ｏ ０３を主成分とするもの）粉
末にニッケルを添加するが、この方法としては、ニッケ
ルを含有する水溶性化合物、例えば硝酸ニッケルを水に
溶解させて得られる水溶液を酸化モリブデン粉末にふり
かけて充分混合し、乾燥させる方法がある。添加するニ
ッケルの量は、０．００２５〜０．０３％（重量％、以
下同じ）とするのが好ましく、０．００５〜０．０３％
とするのがより好ましい、ニッケルの量が０．００２５
％より少ないと、所望の効果を得ることができず、０．
０３％よりも多いと焼結後の加工がきわめて困難となる
。First, nickel is added to the raw material molybdenum oxide (M o Ox, usually molybdenum trioxide M o 03 as the main component) powder. There is a method in which an aqueous solution obtained by dissolving molybdenum oxide in water is sprinkled onto molybdenum oxide powder, thoroughly mixed, and then dried. The amount of nickel added is preferably 0.0025 to 0.03% (wt%, same hereinafter), and 0.005 to 0.03%.
More preferably, the amount of nickel is 0.0025
If it is less than 0.0%, the desired effect cannot be obtained.
If the amount exceeds 0.3%, processing after sintering becomes extremely difficult.
所定量のニッケルを添加した粉末は、水素雰囲気の還元
炉を用いて１段還元を行なう、この還元は１例えば、６
００〜８００ｇの粉末をポートに入れ、５５０℃程度の
低温から１１５０℃程度の高温まで、出口側の温度が次
第に高くなるように温度勾配のついた電気炉中を一定の
速度で進行させる方法で行なう、炉中での保持時間は、
３時間以上とするのが好ましい。The powder to which a predetermined amount of nickel has been added is subjected to one-stage reduction using a reduction furnace in a hydrogen atmosphere.
In this method, 00 to 800 g of powder is put into a port and moved at a constant speed through an electric furnace with a temperature gradient such that the temperature on the exit side gradually increases from a low temperature of about 550 °C to a high temperature of about 1150 °C. The holding time in the furnace is
It is preferable to set it as 3 hours or more.
この還元によって、ブレーン空気透過法による比表面積
が大きい（粒度が細かい）モリブデン金属粉末が得られ
る。このように、１段還元で微細な粉末が得られるのは
、モリブデン中に微量に添加されているニッケルが、還
元中に活性化の働きをなすからであろうと推測される。This reduction yields a molybdenum metal powder with a large specific surface area (fine particle size) by Blaine air permeation method. It is presumed that the reason why a fine powder is obtained in the one-stage reduction is that the trace amount of nickel added to the molybdenum acts as an activator during the reduction.
なお、この製法で得られるモリブデン粉末を加圧成形し
て得られる圧粉体を常法に従って通電焼結した結果１通
常の２段還元で得られるものと同様な高比重の焼結体を
得ることができた。Furthermore, as a result of electrification sintering of the powder compact obtained by pressure-molding the molybdenum powder obtained by this manufacturing method according to a conventional method, a sintered compact with a high specific gravity similar to that obtained by ordinary two-stage reduction is obtained. I was able to do that.
（実施例および比較例）
ニッケルノ添加量が０．００５駕（Ａ） 、 ０．００
２５％（Ｂ） 、 ０．００１７％（Ｃ）の３種の酸化
モリブデン粉末（Ｍ ｏ ０３が主成分）と、ニッケル
を添加しない同様な酸化モリブデン粉末（Ｄ）を、入口
側から順に５５０−８５０−１０５０−１１５０℃と次
第に高温となるように配置された４つのヒートゾーンを
そなえた水素炉で還元した。還元は、ステンレス鋼製の
ポートに酸化物粉末を入れ、該ボートを３５分ごとにそ
の１本分（１つのヒートゾーンに対応）だけ高温側へ移
動させることによって行なった。水素流量はいずれも４
ｍ″／Ｈｒであり、ボートに対する粉末充填量は、上記
Ａ、Ｂ、Ｄが７３０ｇ、 Ｃが８００ｇであった−
この還元によって得られた金属粉末の比表面積Ｓｓと、
この粉末を加圧成形した圧粉体を最高電流４．８０ＯＡ
で通電焼結した場合の比重（計算比重）ＳＧは第１図に
示すようであった。なお、棒状の焼結体の両端部は細く
しであるので、実際の比重は図示されているものより０
．２程度大きくなる。(Example and Comparative Example) The amount of nickel added is 0.005 (A), 0.00
Three types of molybdenum oxide powder (mainly composed of Mo03) of 25% (B) and 0.0017% (C), and a similar molybdenum oxide powder (D) without the addition of nickel, were added in order from the inlet side to 550- Reduction was carried out in a hydrogen furnace equipped with four heat zones arranged to gradually increase the temperature to 850-1050-1150°C. Reduction was accomplished by placing oxide powder in a stainless steel port and moving the boat one boat length (corresponding to one heat zone) to the hot side every 35 minutes. The hydrogen flow rate is 4 in both cases.
m''/Hr, and the amount of powder packed into the boat was 730 g for A, B, and D, and 800 g for C. - The specific surface area Ss of the metal powder obtained by this reduction,
The maximum current of the green compact obtained by pressure molding this powder is 4.80OA.
The specific gravity (calculated specific gravity) SG when electrically sintered was as shown in FIG. In addition, since both ends of the rod-shaped sintered body are tapered, the actual specific gravity is 0.
．． It becomes about 2 times larger.
同図かられかるように、本発明の実施例であるＡ、Ｂは
、ニッケルを添加しないもの（Ｄ）およびニッケル量の
少ないものに較べて、粉末粒度が細かく、焼結したとき
に高比重が得られる。As can be seen from the figure, Examples A and B of the present invention have finer powder particle size and higher specific gravity when sintered than those without nickel (D) and those with a small amount of nickel. is obtained.
（効果）
以上に説明した如く、本発明にかかるモリブデン粉末の
製法は、１段の還元で、粒度が細かく、焼結後に高比重
の得られる粉末を得ることのできるすぐれたものとなっ
た。(Effects) As explained above, the method for producing molybdenum powder according to the present invention is excellent in that it is possible to obtain powder with fine particle size and high specific gravity after sintering through one-stage reduction.
第１図は金属モリブデン粉末の比表面積と焼結後の比重
をあられすグラフである。FIG. 1 is a graph showing the specific surface area and specific gravity of metal molybdenum powder after sintering.
Claims (1)
した酸化モリブデン粉末を水素雰囲気中で低温から徐々
に１０００℃以上の高温に加熱し、酸化モリブデン粉末
を還元して微量のニッケルを含有する金属モリブデン粉
末を得ることを特徴とするモリブデン粉末の製法。(1) Molybdenum oxide powder to which 0.0025 to 0.03% by weight of nickel has been added is gradually heated from a low temperature to a high temperature of 1000°C or higher in a hydrogen atmosphere, and the molybdenum oxide powder is reduced to contain a trace amount of nickel. A method for producing molybdenum powder, which is characterized by obtaining a metallic molybdenum powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4151885A JPS61201708A (en) | 1985-03-01 | 1985-03-01 | Manufacture of molybdenum powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4151885A JPS61201708A (en) | 1985-03-01 | 1985-03-01 | Manufacture of molybdenum powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61201708A true JPS61201708A (en) | 1986-09-06 |
| JPH0543761B2 JPH0543761B2 (en) | 1993-07-02 |
Family
ID=12610593
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4151885A Granted JPS61201708A (en) | 1985-03-01 | 1985-03-01 | Manufacture of molybdenum powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61201708A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7276102B2 (en) | 2004-10-21 | 2007-10-02 | Climax Engineered Materials, Llc | Molybdenum metal powder and production thereof |
| US7524353B2 (en) | 2004-10-21 | 2009-04-28 | Climax Engineered Materials, Llc | Densified molybdenum metal powder and method for producing same |
| CN109848431A (en) * | 2019-02-27 | 2019-06-07 | 金堆城钼业股份有限公司 | A kind of preparation method of thin molybdenum powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5835561A (en) * | 1981-08-26 | 1983-03-02 | Fuji Xerox Co Ltd | Device for preventing contamination of optical system in copying machine |
-
1985
- 1985-03-01 JP JP4151885A patent/JPS61201708A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5835561A (en) * | 1981-08-26 | 1983-03-02 | Fuji Xerox Co Ltd | Device for preventing contamination of optical system in copying machine |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7276102B2 (en) | 2004-10-21 | 2007-10-02 | Climax Engineered Materials, Llc | Molybdenum metal powder and production thereof |
| US7524353B2 (en) | 2004-10-21 | 2009-04-28 | Climax Engineered Materials, Llc | Densified molybdenum metal powder and method for producing same |
| US7785390B2 (en) | 2004-10-21 | 2010-08-31 | Climax Engineered Materials, Llc | Molybdenum metal powder and production thereof |
| US8043406B2 (en) | 2004-10-21 | 2011-10-25 | Climax Engineered Materials, Llc | Molybdenum metal powder |
| US8043405B2 (en) | 2004-10-21 | 2011-10-25 | Climax Engineered Materials, Llc | Densified molybdenum metal powder |
| US8147586B2 (en) | 2004-10-21 | 2012-04-03 | Climax Engineered Materials, Llc | Method for producing molybdenum metal powder |
| CN109848431A (en) * | 2019-02-27 | 2019-06-07 | 金堆城钼业股份有限公司 | A kind of preparation method of thin molybdenum powder |
| CN109848431B (en) * | 2019-02-27 | 2022-05-10 | 金堆城钼业股份有限公司 | Preparation method of fine molybdenum powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0543761B2 (en) | 1993-07-02 |
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