JPH11199948A - Low-temperature-ductile material - Google Patents
Low-temperature-ductile materialInfo
- Publication number
- JPH11199948A JPH11199948A JP10000766A JP76698A JPH11199948A JP H11199948 A JPH11199948 A JP H11199948A JP 10000766 A JP10000766 A JP 10000766A JP 76698 A JP76698 A JP 76698A JP H11199948 A JPH11199948 A JP H11199948A
- Authority
- JP
- Japan
- Prior art keywords
- temperature
- low
- powder
- ductile material
- ductile
- 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
- 239000000463 material Substances 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 36
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011230 binding agent Substances 0.000 claims abstract description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 12
- 239000011733 molybdenum Substances 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 230000007704 transition Effects 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- 239000003870 refractory metal Substances 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 abstract description 4
- 238000005469 granulation Methods 0.000 abstract description 4
- 230000003179 granulation Effects 0.000 abstract description 4
- 229920001223 polyethylene glycol Polymers 0.000 abstract description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 abstract description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 abstract description 3
- 239000010937 tungsten Substances 0.000 abstract description 3
- 238000005238 degreasing Methods 0.000 abstract description 2
- 229910052702 rhenium Inorganic materials 0.000 abstract description 2
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052715 tantalum Inorganic materials 0.000 abstract description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000000758 substrate Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、低温延性材料に係
り、特に、炉用部材、半導体基板、その他構造用部材に
使用される低温延性材料に関する。The present invention relates to a low-temperature ductile material, and more particularly to a low-temperature ductile material used for furnace members, semiconductor substrates, and other structural members.
【０００２】[0002]
【従来の技術】モリブデン、タングステン等の高融点金
属材料は、一般に溶解法による製造が困難であるため、
通常、粉末冶金法により製造される。その製造手順は次
の通りである。2. Description of the Related Art Refractory metal materials such as molybdenum and tungsten are generally difficult to produce by a melting method.
Usually, it is manufactured by a powder metallurgy method. The manufacturing procedure is as follows.
【０００３】まず粒径２〜３μｍ程度のモリブデン粉末
を用意し、これを金型に充填して圧縮成形により所定の
形状に成形する。次いで、この成形体を１８００℃程度
の融点より低い温度で焼結する。次に、得られた焼結体
を圧延して塑性加工することにより、延性脆性遷移温度
（ＤＢＴＴ）を下げ、その後、二次加工を施すことによ
り、製品を得ていた。この場合、ＤＢＴＴを下げるに
は、５０％以上の加工率による塑性加工が必要であると
されていた。また、粉末の成形を自動プレス機で行う場
合、粉末の流動性が悪く、操作性に問題があるため、効
率のよい成形を行うことが困難であった。[0003] First, a molybdenum powder having a particle size of about 2 to 3 µm is prepared, filled in a mold, and formed into a predetermined shape by compression molding. Next, the compact is sintered at a temperature lower than the melting point of about 1800 ° C. Next, the obtained sintered body was rolled and plastically processed to lower the ductile brittle transition temperature (DBTT), and then subjected to secondary processing to obtain a product. In this case, in order to lower the DBTT, it was considered that plastic working at a working ratio of 50% or more was required. In addition, when the powder is formed by an automatic press machine, the flowability of the powder is poor and there is a problem in operability, so that it has been difficult to perform efficient forming.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、このような
事情の下になされ、塑性加工を行うことなく、低温で延
性を示す低温延性材料を提供することを目的とする。本
発明の他の目的は、そのような低温延性材料を製造する
方法を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a low-temperature ductile material which exhibits ductility at a low temperature without performing plastic working under such circumstances. Another object of the present invention is to provide a method for producing such a low temperature ductile material.
【０００５】[0005]
【課題を解決するための手段】上記課題を解決するた
め、本発明（請求項１）は、高融点金属粉末をバインダ
を用いて造粒し、この造粒粉を成形および焼結してなる
高融点金属焼結体からなり、１００℃以下の延性脆性遷
移温度を有することを特徴とする低温延性材料を提供す
る。To solve the above problems, the present invention (claim 1) comprises granulating a high melting point metal powder using a binder, and molding and sintering the granulated powder. Provided is a low-temperature ductile material comprising a refractory metal sintered body and having a ductile brittle transition temperature of 100 ° C. or less.
【０００６】本発明（請求項２）は、上記低温延性材料
（請求項１）において、３５℃以下の延性脆性遷移温度
を有することを特徴とする。本発明（請求項３）は、上
記低温延性材料（請求項１）において、高融点金属はモ
リブデンであることを特徴とする。The present invention (Claim 2) is characterized in that the low-temperature ductile material (Claim 1) has a ductile brittle transition temperature of 35 ° C. or less. The present invention (Claim 3) is characterized in that in the low-temperature ductile material (Claim 1), the high melting point metal is molybdenum.
【０００７】本発明（請求項４）は、高融点金属粉末を
バインダを用いて造粒する工程、得られた造粒粉を成形
する工程、および得られた成形体を焼結する工程を具備
し、１００℃以下の延性脆性遷移温度を有することを特
徴とする低温延性材料の製造方法を提供する。The present invention (claim 4) comprises a step of granulating a high melting point metal powder using a binder, a step of forming the obtained granulated powder, and a step of sintering the obtained formed body. The present invention also provides a method for producing a low-temperature ductile material, which has a ductile brittle transition temperature of 100 ° C. or less.
【０００８】本発明（請求項５）は、上記低温延性材料
の製造方法（請求項４）において、高融点金属はモリブ
デンであることを特徴とする。本発明（請求項６）は、
上記低温延性材料の製造方法（請求項４）において、造
粒粉は２０〜１００μｍの平均粒径を有することを特徴
とする。The present invention (Claim 5) is characterized in that, in the method for producing a low-temperature ductile material (Claim 4), the high melting point metal is molybdenum. The present invention (claim 6)
In the method for producing a low-temperature ductile material (claim 4), the granulated powder has an average particle diameter of 20 to 100 μm.
【０００９】以上のように構成される本発明の低温延性
材料は、高融点金属粉末の粉末冶金法により製造され
る。高融点金属粉末としては、モリブデン、タングステ
ン、タンタル、レニウム等が用いられる。高融点金属粉
末の粒径は、１〜５μｍであるのが好ましい。[0009] The low-temperature ductile material of the present invention configured as described above is manufactured by powder metallurgy of a high melting point metal powder. As the high melting point metal powder, molybdenum, tungsten, tantalum, rhenium or the like is used. The particle size of the high melting point metal powder is preferably 1 to 5 μm.
【００１０】本発明の低温延性材料の製造においては、
従来と異なり、高融点金属粉末を造粒して造粒粉を形成
する。造粒は、高融点金属粉末にバインダ−を添加して
行われる。バインダ−としては、ポリビニルアルコ−
ル、ポリエチレングリコ−ル等を用いることができる。
高融点金属粉末とバインダ−との混合割合は、２００：
１〜５０：１が好ましい。また、得られた造粒粉の粒径
は、２０〜１００μｍであるのが好ましい。In the production of the low-temperature ductile material of the present invention,
Unlike the conventional method, a high melting point metal powder is granulated to form a granulated powder. Granulation is performed by adding a binder to the high melting point metal powder. As the binder, polyvinyl alcohol
And polyethylene glycol can be used.
The mixing ratio of the high melting point metal powder and the binder is 200:
1-50: 1 is preferred. The particle size of the obtained granulated powder is preferably 20 to 100 μm.
【００１１】造粒粉の粒径が２０μｍ未満では、造粒粉
の流動性が悪化し、均一な成形体が得られなくなり、一
方、１００μｍを越えると、造粒粉の造粒が困難とな
り、好ましくない。より好ましくは４０〜７０μｍであ
る。When the particle size of the granulated powder is less than 20 μm, the fluidity of the granulated powder is deteriorated and a uniform molded body cannot be obtained. On the other hand, when it exceeds 100 μm, granulation of the granulated powder becomes difficult, Not preferred. More preferably, it is 40 to 70 μm.
【００１２】次に、造粒粉は所定のサイズおよび形状に
成形される。成形圧力は、１〜４ｋｇ／ｃｍ2 程度が好
ましい。得られた成形体は、その後、脱脂され、更に焼
結される。脱脂は、６００〜９００℃の温度で２〜５時
間、焼結は、１７００〜１９００℃の温度で５〜１０時
間、行うことが好ましい。焼結を過度に長時間行うと、
後述するように、低温延性に影響を与える因子の１つと
考えられるバインダ−中のカ−ボンが少なくなり過ぎて
しまうため、好ましくない。Next, the granulated powder is formed into a predetermined size and shape. The molding pressure is preferably about 1 to 4 kg / cm 2 . The obtained molded body is thereafter degreased and further sintered. Degreasing is preferably performed at a temperature of 600 to 900 ° C for 2 to 5 hours, and sintering is preferably performed at a temperature of 1700 to 1900 ° C for 5 to 10 hours. If sintering is performed for an excessively long time,
As will be described later, the amount of carbon in the binder, which is considered to be one of the factors affecting low-temperature ductility, is undesirably reduced.
【００１３】以上のようにして得られた焼結体は、所定
の形状に加工されて、炉用部材、整流素子用基板、半導
体基板、その他構造用部材等の製品とされる。以上説明
した本発明の低温延性材料は、１００℃以下の延性脆性
遷移温度を有するという、低温で優れた延性を有する。
本発明の低温延性材料がこのように低温で優れた延性を
有する理由は、未だ明確ではないが、恐らく、従来の材
料とは異なり、造粒粉を成形・焼結していることから、
造粒工程、例えばバインダ−の使用が何らかの形で関与
していることが考えられる。The sintered body obtained as described above is processed into a predetermined shape to obtain products such as furnace members, rectifying element substrates, semiconductor substrates, and other structural members. The low-temperature ductile material of the present invention described above has excellent ductility at low temperatures, having a ductile-brittle transition temperature of 100 ° C. or less.
The reason why the low-temperature ductile material of the present invention has excellent ductility at such a low temperature is not yet clear, but probably, unlike conventional materials, because granulated powder is molded and sintered,
It is possible that the granulation process, for example the use of a binder, is involved in some way.
【００１４】すなわち、バインダ−の使用により導入さ
れたカ−ボンは、一般に、焼結により殆どが除去される
ものと考えられていたが、本発明者らの実験によると、
その半分程度が焼結後も残留していることがわかった。
この焼結体中に残留するカ−ボンが、低温での延性に影
響を与える因子の１つではないかと思われる。That is, it has been generally thought that carbon introduced by the use of a binder is almost completely removed by sintering.
It was found that about half thereof remained after sintering.
It is considered that the carbon remaining in the sintered body is one of the factors affecting the low-temperature ductility.
【００１５】[0015]
【発明の実施の形態】以下、本発明の実施例を示し、本
発明についてより具体的に説明する。 実施例 図１に示す工程に従って、低温延性材料を製造した。ま
ず、粒径２．５μｍのモリブデン粉末３０ｋｇを用意
し、これにバインダ−としてポリビニルアルコ−ル（Ｐ
ＶＡ）およびポリエチレングリコール（ＰＥＧ）のそれ
ぞれ０．３ｋｇを加え、混合し、次いで、スプレ−ドラ
イヤ−により造粒し、粒径５０μｍのモリブデン造粒粉
を得た。このモリブデン造粒粉中のカ−ボン含有量を測
定したところ、３３００ｐｐｍであった。DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be shown, and the present invention will be described more specifically. Example A low-temperature ductile material was manufactured according to the process shown in FIG. First, 30 kg of molybdenum powder having a particle size of 2.5 μm was prepared, and polyvinyl alcohol (P) was used as a binder.
0.3 kg of each of VA) and polyethylene glycol (PEG) were added, mixed, and then granulated by a spray dryer to obtain a molybdenum granulated powder having a particle size of 50 μm. When the carbon content in the molybdenum granulated powder was measured, it was 3300 ppm.
【００１６】次いで、得られたモリブデン造粒粉を１ｔ
／ｃｍ2 、２ｔ／ｃｍ2 、３ｔ／ｃｍ2 、４ｔ／ｃｍ2
の成形圧力により、径８６ｍｍ×厚み３ｍｍの形状に成
形し、４種の成形体を得た。成形機としては、油圧プレ
ス（５００トン）を用いた。この場合、モリブデン造粒
粉は流動性に富んでいるので、成形機への充填をスム−
スに行うことができた。Next, the obtained molybdenum granulated powder was
/ Cm 2 , 2 t / cm 2 , 3 t / cm 2 , 4 t / cm 2
, And formed into a shape having a diameter of 86 mm and a thickness of 3 mm to obtain four types of molded products. A hydraulic press (500 tons) was used as a molding machine. In this case, since the molybdenum granulated powder is rich in fluidity, filling the molding machine is smooth.
Was able to do it.
【００１７】次に、形成体を８５０℃で脱脂し、更に１
７５０℃で７．５時間、焼結し、焼結体を得た。得られ
た４種の焼結体について、密度、カ−ボン残存量（ｐｐ
ｍ）、伸びを測定したところ、下記表に示す結果を得
た。Next, the formed body was degreased at 850 ° C.
Sintering was performed at 750 ° C. for 7.5 hours to obtain a sintered body. Regarding the obtained four types of sintered bodies, the density and the remaining amount of carbon (pp
m) and elongation were measured, and the results shown in the following table were obtained.
【００１８】[0018]
【表１】 [Table 1]
【００１９】上記表から、４種の焼結体は、１〜４ｔ／
ｃｍ2 のいずれの成形圧力によっても、優れた延性を示
していることがわかる。なお、焼結によっても１１０〜
１５５０ｐｐｍのカ−ボンが残存しており、これが延性
に影響を及ぼしていることが考えられる。From the above table, the four types of sintered bodies are 1 to 4 t /
It can be seen that excellent ductility is exhibited at any molding pressure of cm 2 . In addition, 110-110
It is thought that 1550 ppm of carbon remained, which affected ductility.
【００２０】以上のようにして得られた焼結体は、次い
で曲げ加工等の二次加工が施され、所定の製品とされ
る。この場合、焼結体は、低温においても優れた延性を
有するため、曲げ加工等の二次加工を容易に行うことが
可能である。The sintered body obtained as described above is then subjected to secondary processing such as bending to obtain a predetermined product. In this case, since the sintered body has excellent ductility even at a low temperature, it is possible to easily perform secondary processing such as bending.
【００２１】なお、以上の実施例では、高融点金属とし
てモリブデンを用いた場合について説明したが、本発明
は、これに限らず、タングステン、タンタル、レニウム
等の他の高融点金属を用いることも可能であり、また、
これら高融点金属の合金を用いてもよい。In the above embodiments, the case where molybdenum is used as the high melting point metal has been described. Is possible, and
An alloy of these refractory metals may be used.
【００２２】[0022]
【発明の効果】以上説明したように、本発明によれば、
高融点金属粉末をバインダを用いて造粒し、この造粒粉
を成形および焼結してなる高融点金属焼結体により構成
されているため、塑性加工を施すことなく１００℃以下
の延性脆性遷移温度を示すという、極めて優れた低温延
性を示す低温延性材料が得られる。As described above, according to the present invention,
The high melting point metal powder is granulated using a binder, and the granulated powder is formed and sintered to form a high melting point metal sintered body. A low-temperature ductile material that exhibits a transition temperature and exhibits extremely excellent low-temperature ductility is obtained.
【図１】本発明の一実施例に係る低温延性材料の製造工
程を示す工程図。FIG. 1 is a process chart showing a process for producing a low-temperature ductile material according to one embodiment of the present invention.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 湯本 進一 神奈川県横浜市磯子区新杉田町８番地 株 式会社東芝横浜事業所内 (72)発明者 足達 祥卓 神奈川県横浜市磯子区新杉田町８番地 株 式会社東芝横浜事業所内 ──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Shinichi Yumoto 8 Shinsugita-cho, Isogo-ku, Yokohama-shi, Kanagawa Prefecture Inside the Toshiba Yokohama Office (72) Inventor Yoshitaka Adachi 8th Shin-Sugita-cho, Isogo-ku, Yokohama-shi, Kanagawa Toshiba Yokohama Office
Claims (6)
し、この造粒粉を成形および焼結してなる高融点金属焼
結体からなり、１００℃以下の延性脆性遷移温度を有す
ることを特徴とする低温延性材料。1. A high melting metal sintered body obtained by granulating a high melting metal powder using a binder, molding and sintering the granulated powder, and having a ductile brittle transition temperature of 100 ° C. or less. A low-temperature ductile material characterized by the following.
ことを特徴とする請求項１に記載の低温延性材料。2. The low temperature ductile material according to claim 1, having a ductile brittle transition temperature of 35 ° C. or less.
を特徴とする請求項１に記載の低温延性材料。3. The low-temperature ductile material according to claim 1, wherein the refractory metal is molybdenum.
する工程、得られた造粒粉を成形する工程、および得ら
れた成形体を焼結する工程を具備し、１００℃以下の延
性脆性遷移温度を有することを特徴とする低温延性材料
の製造方法。4. A process for granulating a high melting point metal powder using a binder, a step for molding the obtained granulated powder, and a step for sintering the obtained molded body, wherein the ductility is 100 ° C. or less. A method for producing a low-temperature ductile material, characterized by having a brittle transition temperature.
を特徴とする請求項４に記載の低温延性材料の製造方
法。5. The method according to claim 4, wherein the refractory metal is molybdenum.
径を有することを特徴とする請求項４に記載の低温延性
材料の製造方法。6. The method for producing a low-temperature ductile material according to claim 4, wherein the granulated powder has an average particle size of 20 to 100 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10000766A JPH11199948A (en) | 1998-01-06 | 1998-01-06 | Low-temperature-ductile material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10000766A JPH11199948A (en) | 1998-01-06 | 1998-01-06 | Low-temperature-ductile material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11199948A true JPH11199948A (en) | 1999-07-27 |
Family
ID=11482830
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10000766A Pending JPH11199948A (en) | 1998-01-06 | 1998-01-06 | Low-temperature-ductile material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11199948A (en) |
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| WO2012157336A1 (en) * | 2011-05-19 | 2012-11-22 | 株式会社東芝 | Method for producing molybdenum granulated powder, and molybdenum granulated powder |
| WO2012157334A1 (en) * | 2011-05-16 | 2012-11-22 | 株式会社東芝 | Method for producing molybdenum granulated powder, and molybdenum granulated powder |
| WO2012169256A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169262A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169255A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169261A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169258A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
-
1998
- 1998-01-06 JP JP10000766A patent/JPH11199948A/en active Pending
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| CN103476522A (en) * | 2011-05-16 | 2013-12-25 | 株式会社东芝 | Method for producing molybdenum granulated powder, and molybdenum granulated powder |
| WO2012157334A1 (en) * | 2011-05-16 | 2012-11-22 | 株式会社東芝 | Method for producing molybdenum granulated powder, and molybdenum granulated powder |
| JP5917502B2 (en) * | 2011-05-16 | 2016-05-18 | 株式会社東芝 | Method for producing molybdenum granulated powder |
| JPWO2012157334A1 (en) * | 2011-05-16 | 2014-07-31 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012157336A1 (en) * | 2011-05-19 | 2012-11-22 | 株式会社東芝 | Method for producing molybdenum granulated powder, and molybdenum granulated powder |
| JP5917503B2 (en) * | 2011-05-19 | 2016-05-18 | 株式会社東芝 | Method for producing molybdenum granulated powder |
| JPWO2012157336A1 (en) * | 2011-05-19 | 2014-07-31 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169256A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169257A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169258A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169261A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169255A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| WO2012169262A1 (en) * | 2011-06-08 | 2012-12-13 | 株式会社東芝 | Method for producing molybdenum granulated powder and molybdenum granulated powder |
| CN102259189A (en) * | 2011-07-28 | 2011-11-30 | 北京科技大学 | Preparation method of porous cathode substrate |
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