JPH028304A - Manufacture of tungsten powder - Google Patents
Manufacture of tungsten powderInfo
- Publication number
- JPH028304A JPH028304A JP15889488A JP15889488A JPH028304A JP H028304 A JPH028304 A JP H028304A JP 15889488 A JP15889488 A JP 15889488A JP 15889488 A JP15889488 A JP 15889488A JP H028304 A JPH028304 A JP H028304A
- Authority
- JP
- Japan
- Prior art keywords
- reaction
- tungsten
- powder
- gas
- tungsten powder
- 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
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- 238000010574 gas phase reaction Methods 0.000 claims abstract description 7
- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 abstract description 14
- 239000000843 powder Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000005477 sputtering target Methods 0.000 abstract description 4
- 230000015271 coagulation Effects 0.000 abstract 1
- 238000005345 coagulation Methods 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 13
- 229910052721 tungsten Inorganic materials 0.000 description 8
- 239000010937 tungsten Substances 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明はスパッタリングターゲットあるいは導電ペース
ト材料等として有用な高純度タングステン粉末の製造法
に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing high-purity tungsten powder useful as a sputtering target or a conductive paste material.
［従来の技術］
タングステンは高融点で電気抵抗の小さい金属であり、
各種電子材料用素材として金属単体あるいはそのシリサ
イドの形で広く使用されており、特に、スパッタリング
材料として使用されているものであるが、かかる用途に
おいては原料のタングステン粉末として不純物の少ない
粉末、特に酸素含有量の少ないものが要求されるもので
ある。[Prior art] Tungsten is a metal with a high melting point and low electrical resistance.
It is widely used as a material for various electronic materials in the form of simple metal or its silicide, and is particularly used as a sputtering material.In such applications, tungsten powder with low impurities, especially oxygen, is used as the raw material. A low content is required.
また、導電ペースト用としては凝集粉末ではビヒクルと
分離しやすいため、分散性の良好な粉末が要求されるも
のである。また、これらの用途においてはいずれも粒子
が球状に近い方が好ましいものである。Furthermore, for use in conductive pastes, agglomerated powders are easily separated from the vehicle, so powders with good dispersibility are required. Furthermore, in all of these uses, it is preferable that the particles be nearly spherical.
タングステン粉末の製造法としては、パラタングステン
酸アンモニウムの加水分解によって得られるタングステ
ン酸化物を、水素ふん囲気中で還元する方法が一般的で
ある（湿式法と称する）。A common method for producing tungsten powder is to reduce tungsten oxide obtained by hydrolyzing ammonium paratungstate in a hydrogen atmosphere (referred to as a wet method).
かかる方法においては原料、処理薬剤に由来する不純物
が混入し、また、スパッタリングターゲツト材において
は酸素含有量を可及的に少なくしたものが要望されるも
のであるが、通常の処理法では高度な酸素除去は困難で
ある。さらにこのようにして得られる粉末は粒子が凝結
したような状態である。In such methods, impurities derived from raw materials and processing chemicals are mixed in, and it is desired that the sputtering target material has as low an oxygen content as possible; Oxygen removal is difficult. Furthermore, the powder thus obtained is in a state where the particles are agglomerated.
［問題点を解決するための具体的手段］本発明者らはか
かる問題点に鑑み鋭意検討の結果、６フッ化タングステ
ンおよび水素の混合カスを特定の条件のもとて気相反応
させることにより高純度で略球状の単分散タングステン
粉末か得られることを見出し本発明に到達したものであ
る。[Specific means for solving the problem] In view of the problem, the present inventors have conducted intensive studies and found that by causing a gas phase reaction of tungsten hexafluoride and hydrogen mixed residue under specific conditions. The present invention was achieved by discovering that highly pure, substantially spherical, monodisperse tungsten powder can be obtained.
すなわち本発明は６フッ化タンクステン、水素の混合ガ
スをＨ２／ＷＦ６のモル比４以上で６５０〜１４００℃
の範囲で気相反応させることを特徴とするタングステン
粉末の製造法および同様の方法において反応系に不活性
ガスを添加する方法である。That is, in the present invention, a mixed gas of tanksten hexafluoride and hydrogen is heated at 650 to 1400°C at a molar ratio of H2/WF6 of 4 or more.
This is a method for producing tungsten powder characterized by carrying out a gas phase reaction in a range of 100 to 100 ml, and a method for adding an inert gas to the reaction system in a similar method.
本発明においてはＨ２／ＷＦ６のモル比を４以上とし、
反応温度を６５０〜１４００°Ｃの範囲とするものであ
り、モル比かこれより小さい場合には、生成タングステ
ン粉末の粒径が不揃いとなるほがＷＦ６が一部未反応の
まま排出されることとなり好ましくない。また、この温
度より低い温度ては原料６フッ化タングステンの量に対
して、反応装置壁面が十分に広い場合には、この壁面で
反応が進行し、タングステン膜を形成するが、原料６フ
ッ化タングステンの量に対して、反応装置壁面が十分に
広くない場合には、はとんどの６フッ化タングステンは
未反応のまま反応系外へ排出される。In the present invention, the molar ratio of H2/WF6 is set to 4 or more,
The reaction temperature is set in the range of 650 to 1400°C, and if the molar ratio is smaller than this, the particle size of the produced tungsten powder will be uneven, and some of the WF6 will be discharged unreacted. This is undesirable. In addition, at a temperature lower than this temperature, if the wall surface of the reactor is sufficiently wide relative to the amount of raw material tungsten hexafluoride, the reaction proceeds on this wall surface and forms a tungsten film, but the raw material tungsten hexafluoride If the wall surface of the reactor is not wide enough for the amount of tungsten, most of the tungsten hexafluoride will be discharged from the reaction system unreacted.
反応温度は基本的にはこの温度以上であれば構わないが
、１４００℃程度で十分な反応速度を有するため、特に
これ以上にしても利点はない。かがる観点からより好ま
しい反応条件としてはＨ２／ＷＦ６のモル比が６〜５０
で、反応温度７００〜１２００℃が推奨される。The reaction temperature basically does not matter as long as it is higher than this temperature, but since the reaction rate is sufficient at about 1400° C., there is no particular advantage in setting it higher than this temperature. From the viewpoint of darkening, more preferable reaction conditions include a H2/WF6 molar ratio of 6 to 50.
Therefore, a reaction temperature of 700 to 1200°C is recommended.
反応圧力は特に限定されないが減圧系では生成タングス
テン粒径が小さくなるという傾向がありまた、若干加圧
系では粒径が大きくなるという傾向があり、−船釣には
１００ Ｔｏｒｒ〜１．５ ａｔｍの範囲が推奨され、
特に装置、操作の簡便さ等がら大気圧が最も好ましい。Although the reaction pressure is not particularly limited, there is a tendency for the particle size of generated tungsten to become smaller in a reduced pressure system, and a tendency for the particle size to become larger in a slightly pressurized system.-100 Torr to 1.5 atm for boat fishing A range of is recommended;
In particular, atmospheric pressure is most preferred in view of ease of equipment and operation.
このようにして得られるタングステン粉末は反応条件に
もよるが０．１〜２０μｒｎ程度の粒径を有する単分散
粒子てあり、その形状は略球状を呈するものである。The tungsten powder thus obtained is a monodisperse particle having a particle size of about 0.1 to 20 μrn, depending on the reaction conditions, and its shape is approximately spherical.
６フッ化タングステンおよび水素以外に不活性カスを反
応系に加えた場合には、得られるタングステン粉末の形
状はさらに球に近くなるものである。不活性ガスを添加
した場合になぜ得られるタングステン粉末が球状となる
のが、球状化効果の理由は定かではないがその効果は顕
著である。ここでいう不活性ガスとは、本発明の反応温
度範囲内で原料カスと反応しないガスを指すものであり
、アルゴン、ヘリウムのような稀ガスあるいはＣＦ４等
の化学的に安定な化合物ガス等が挙げられる。When inert scum is added to the reaction system in addition to tungsten hexafluoride and hydrogen, the shape of the resulting tungsten powder becomes even more spherical. The reason why the tungsten powder obtained becomes spherical when an inert gas is added is not clear, but the effect is remarkable. The inert gas here refers to a gas that does not react with the raw material residue within the reaction temperature range of the present invention, and includes rare gases such as argon and helium, or chemically stable compound gases such as CF4. Can be mentioned.
不活性ガスの添加量は原料６フッ化タングステン量に対
してモル比で２倍以上が好ましく、これより少ない場合
には、生成粒子に対する球状化効果が少なく、また、Ｈ
２に対してモル比で２倍以上では原料カス濃度の低下を
招き装置効率が悪くなる。また、用いる不活性ガスの種
類としてはアルゴンガスが最も経済的てあり、推奨され
る。The amount of inert gas added is preferably at least twice the molar ratio of the amount of tungsten hexafluoride as the raw material.
If the molar ratio is more than 2 times that of 2, the concentration of raw material residue will decrease and the efficiency of the device will deteriorate. Furthermore, as the type of inert gas to be used, argon gas is the most economical and is recommended.
不活性ガスの添加以外に反応ガスの線速度を大きくする
ことによっても球状化の効果が認められるが、不活性ガ
スを添加する場合はさらにその効果は大きい。In addition to the addition of an inert gas, the effect of spheroidization can also be observed by increasing the linear velocity of the reaction gas, but the effect is even greater when an inert gas is added.
反応装置としては特に制限されないが、生成タングステ
ン粉末の捕集のし易さ等がら縦形の反応器が有利である
。粒径の比較的大きいタングステン粉末を得たい場合に
はタングステンの比重が大きいことから原料ガスを反応
管の上部に導入し、反応管の上部から下部方向に流し反
応させ、反応により生成するタングステン粉末を反応管
の下方に設けたタングステン粉末捕集器にて捕集する。The reactor is not particularly limited, but a vertical reactor is advantageous in view of ease of collecting the produced tungsten powder. If you want to obtain tungsten powder with a relatively large particle size, the raw material gas is introduced into the upper part of the reaction tube, flows from the upper part to the lower part of the reaction tube, and the tungsten powder produced by the reaction is produced. is collected by a tungsten powder collector installed below the reaction tube.
一方、微細なタングステン粉末を得たい場合には反応管
下部がら原料ガスを導入し、下部から上部にガスを流し
て反応させ、反応管の上方に設けたタングステン粉末捕
集器にて捕集する。On the other hand, if you want to obtain fine tungsten powder, the raw material gas is introduced from the bottom of the reaction tube, the gas is allowed to flow from the bottom to the top and reacted, and then collected by a tungsten powder collector installed above the reaction tube. .
原料ガス導入にあたっては６フッ化タングステンと水素
を別々に導入する方法と混合して導入する方法があるが
、予め混合して導入する場合、ノズル付近は十分に高温
とはいえず、ノズル内あるいはノズル周辺で原料が反応
し、膜の状態で厚み方向へ成長し、ノズルの閉塞の原因
となることもある。また、本発明の反応においては反応
温度が高いほど得られるタングステン粉末は小さくなる
傾向があるため、微細なタングステン粉末を得たい場合
には予め混合して導入するよりも別々に導入し、高温の
反応ゾーンで瞬時に反応させることが好ましい。大きい
タングステン粉末を得たい場合にはこの逆をおこなえは
よく、反応温度自体を低く、また、水素に対する６フッ
化タングステンの量を大きくするほどより大きいタング
ステン粉末が得られる。このようにして得られるタング
ステン粉末中の酸素含有量は２ｏｐｐｍ以下と極めてす
くないものである。When introducing raw material gas, there are two methods: introducing tungsten hexafluoride and hydrogen separately and introducing them together. However, when introducing them together in advance, the temperature near the nozzle is not sufficiently high, and the inside of the nozzle or The raw material reacts around the nozzle and grows in the thickness direction in the form of a film, which may cause the nozzle to become clogged. In addition, in the reaction of the present invention, the higher the reaction temperature, the smaller the tungsten powder obtained, so if you want to obtain fine tungsten powder, it is better to introduce it separately rather than mixing it in advance. It is preferable to react instantly in the reaction zone. If it is desired to obtain a large tungsten powder, the reverse can be done; the lower the reaction temperature itself and the larger the amount of tungsten hexafluoride relative to hydrogen, the larger the tungsten powder obtained. The oxygen content in the tungsten powder obtained in this way is extremely low, 2 oppm or less.
反応管の材質はカーホンが好ましい。耐熱合金等も使用
し得るが、還元雰囲気て、ＷＦ６および副生ＨＦによる
腐食（表面反応）により、製品タングステン中に微量の
不純物が混入することとなり、極めて高純度のタングス
テン粉末を得たい場合には適当てはない。また、カーボ
ンは気密性が十分でないためその表面をタングステンコ
ーティングすることが好ましい。コーティングの手段と
して６フッ化タンクステンと水素との気相反応蒸着が適
当である。The material of the reaction tube is preferably carphone. Heat-resistant alloys can also be used, but in a reducing atmosphere, corrosion (surface reaction) caused by WF6 and by-product HF will cause trace amounts of impurities to be mixed into the product tungsten, so if you want to obtain extremely high-purity tungsten powder, is not appropriate. Further, since carbon does not have sufficient airtightness, it is preferable to coat the surface with tungsten. Vapor phase reactive deposition of tanksten hexafluoride and hydrogen is suitable as a means of coating.
以下、本発明を実施例により具体的に説明する。Hereinafter, the present invention will be specifically explained with reference to Examples.
実施例１〜６、比較例１〜３
６フッ化タングステン、水素の気相反応により表面にタ
ングステンコーティングを施した内径５０ＩｎＩ１１、
長さ１０００ｍｍのカーボン製反応管を具備した縦型反
応装置を用い、反応管上部から原料ガスを別々に導入し
、原料ガス流量、反応温度、反応圧力、滞在時間を第１
表のとおりとして反応をおこなった。この結果を第１表
に示した。また、実施例２および実施例３で得たタング
ステン粉末の粒子構造のＳＥＭ写真を第１図および第２
図に示した。Examples 1 to 6, Comparative Examples 1 to 3 Inner diameter 50 InI11 with tungsten coating applied to the surface by gas phase reaction of tungsten hexafluoride and hydrogen,
Using a vertical reactor equipped with a 1000 mm long carbon reaction tube, raw material gases are introduced separately from the upper part of the reaction tube, and the raw material gas flow rate, reaction temperature, reaction pressure, and residence time are
The reaction was carried out as shown in the table. The results are shown in Table 1. In addition, SEM photographs of the particle structures of the tungsten powders obtained in Example 2 and Example 3 are shown in Figures 1 and 2.
Shown in the figure.
また、湿式法で得られた市販タングステン粉末（比較例
１）の不純物含有量、粒径を第１表に、ＳＥＭ写真を第
３図に示した。Further, the impurity content and particle size of the commercially available tungsten powder (Comparative Example 1) obtained by the wet method are shown in Table 1, and the SEM photograph is shown in FIG.
［発明の効果］
本発明によれば高純度、特に酸素含有量が極めて少ない
タングステン粉末を容易に得ることができ、得られる粉
末は凝集性のない単分散粒子であり、その形状も球状で
あるなめ、スパッタリングターゲット用とした場合焼結
性が良好であり、また、導電ペースト用とした場合には
分散性が非常によいものである。[Effects of the Invention] According to the present invention, it is possible to easily obtain tungsten powder with high purity, especially with extremely low oxygen content, and the obtained powder is monodisperse particles without agglomeration, and its shape is also spherical. It has good sinterability when used as a sputtering target, and has very good dispersibility when used as a conductive paste.
第１図、第２図、第３図はそれぞれ実施例２、実施例３
および市販のタングステン粉末の粒子構造のＳＥＭ写真
を示すものである。
特許出願人 セントラル硝子株式会社
第１図
第２図
１０μｍ
第３図
１０μｍFigures 1, 2, and 3 are Example 2 and Example 3, respectively.
and SEM photographs of the particle structure of commercially available tungsten powder. Patent applicant Central Glass Co., Ltd. Figure 1 Figure 2 10μm Figure 3 10μm
Claims (2)
／ＷＦ＿６のモル比４以上、反応温度６５０〜１４００
℃の範囲で気相反応させることを特徴とするタングステ
ン粉末の製造法。(1) Mixed gas of tungsten hexafluoride and hydrogen to H_2
/WF_6 molar ratio 4 or more, reaction temperature 650-1400
A method for producing tungsten powder characterized by carrying out a gas phase reaction in the temperature range.
混合ガスをＨ＿２／ＷＦ＿６のモル比４以上で６５０〜
１４００℃の範囲で気相反応させることを特徴とするタ
ングステン粉末の製造法。(2) Mixed gas of tungsten hexafluoride, hydrogen and inert gas at a molar ratio of H_2/WF_6 of 4 or more from 650 to 650
A method for producing tungsten powder, characterized by carrying out a gas phase reaction in a range of 1400°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15889488A JPH028304A (en) | 1988-06-27 | 1988-06-27 | Manufacture of tungsten powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15889488A JPH028304A (en) | 1988-06-27 | 1988-06-27 | Manufacture of tungsten powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH028304A true JPH028304A (en) | 1990-01-11 |
Family
ID=15681701
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15889488A Pending JPH028304A (en) | 1988-06-27 | 1988-06-27 | Manufacture of tungsten powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH028304A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100494976B1 (en) * | 2002-08-29 | 2005-06-13 | 한국기계연구원 | Process for manufacturing WC based powder by vapor reaction under atmospheric pressure |
| WO2006098781A2 (en) * | 2005-03-11 | 2006-09-21 | Honeywell International Inc. | Methods for making sputtering targets |
| CN104174862A (en) * | 2014-07-21 | 2014-12-03 | 北京科技大学 | Preparation method of spherical tungsten powder |
| KR101699881B1 (en) * | 2015-08-13 | 2017-01-25 | 서울대학교산학협력단 | Method for preparing monodisperse metal fine particles |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5031554A (en) * | 1973-07-20 | 1975-03-28 |
-
1988
- 1988-06-27 JP JP15889488A patent/JPH028304A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5031554A (en) * | 1973-07-20 | 1975-03-28 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100494976B1 (en) * | 2002-08-29 | 2005-06-13 | 한국기계연구원 | Process for manufacturing WC based powder by vapor reaction under atmospheric pressure |
| WO2006098781A2 (en) * | 2005-03-11 | 2006-09-21 | Honeywell International Inc. | Methods for making sputtering targets |
| WO2006098781A3 (en) * | 2005-03-11 | 2006-11-09 | Honeywell Int Inc | Methods for making sputtering targets |
| CN104174862A (en) * | 2014-07-21 | 2014-12-03 | 北京科技大学 | Preparation method of spherical tungsten powder |
| CN104174862B (en) * | 2014-07-21 | 2016-08-17 | 北京科技大学 | A kind of preparation method of globular tungsten powder |
| KR101699881B1 (en) * | 2015-08-13 | 2017-01-25 | 서울대학교산학협력단 | Method for preparing monodisperse metal fine particles |
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