JP2002327265A - High purity ruthenium target and manufacturing method therefor - Google Patents
High purity ruthenium target and manufacturing method thereforInfo
- Publication number
- JP2002327265A JP2002327265A JP2001131378A JP2001131378A JP2002327265A JP 2002327265 A JP2002327265 A JP 2002327265A JP 2001131378 A JP2001131378 A JP 2001131378A JP 2001131378 A JP2001131378 A JP 2001131378A JP 2002327265 A JP2002327265 A JP 2002327265A
- Authority
- JP
- Japan
- Prior art keywords
- purity
- ruthenium
- target
- purity ruthenium
- less
- 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
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 68
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 238000005477 sputtering target Methods 0.000 abstract description 18
- 238000010894 electron beam technology Methods 0.000 description 18
- 238000004090 dissolution Methods 0.000 description 11
- 238000005242 forging Methods 0.000 description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 description 8
- 238000005096 rolling process Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 238000009924 canning Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005058 metal casting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、５Ｎ（９９．９
９９ｗｔ％）レベル以上の均一な鍛造組織を有する高純
度ルテニウムスパッタリングターゲット及び３Ｎ（９
９．９ｗｔ％）レベルの比較的低純度のルテニウム粉末
を使用して５レベル以上の均一な鍛造組織を有する高純
度ルテニウムスパッタリングターゲットを割れを発生さ
せずに安定して製造できる方法に関する。TECHNICAL FIELD The present invention relates to a 5N (99.9)
High-purity ruthenium sputtering target having a uniform forged structure of not less than 99 wt%) and 3N (9
The present invention relates to a method for stably producing a high-purity ruthenium sputtering target having a uniform forging structure of 5 levels or more using a relatively low-purity ruthenium powder (9.9 wt%) without causing cracks.
【０００２】[0002]
【従来の技術】近年、高純度のルテニウムは、強誘電体
電極等のエレクトロニクス材料又は触媒やその他の加工
用原料として使用されているが、一般にルテニウム薄膜
を形成する場合にはスパッタリング法を用いることが多
い。スパッタリング法自体は、エレクトロニクス分野に
おいてよく知られた方法であるが、このスパッタリング
に適合する均一でかつ安定した特性を持つ高純度ルテニ
ウムターゲットが要求されている。一般に、市販されて
いる比較的純度の高いルテニウム材料は３Ｎレベルの粉
末である。しかし、最近のエレクトロニクス分野で使用
される材料は、ノイズ発生を防止し、特性を向上させる
目的から、さらに高純度化が要求されており、高純度ル
テニウムスパッタリングターゲットとしても純度５Ｎレ
ベルが必要とされている。2. Description of the Related Art In recent years, high-purity ruthenium has been used as an electronic material such as a ferroelectric electrode, a catalyst, or other raw material for processing. In general, when a ruthenium thin film is formed, a sputtering method is used. There are many. Although the sputtering method itself is a well-known method in the field of electronics, a high-purity ruthenium target having uniform and stable characteristics suitable for the sputtering is required. Generally, commercially available relatively pure ruthenium materials are 3N level powders. However, materials used in the recent electronics field are required to be further purified for the purpose of preventing noise generation and improving characteristics, and a high purity ruthenium sputtering target is required to have a purity level of 5N. ing.
【０００３】以上から、市販されている３Ｎレベルのル
テニウム粉末を使用して、この粉末の純度をさらに向上
させ、かつスパッタリングターゲットに加工する必要が
ある。しかし、低い純度のルテニウム粉末をアーク溶解
等により不純物を揮発させて純度を高めた金属ルテニウ
ムの溶解鋳造品（インゴット）は、硬くかつ脆いため通
常の圧延や鍛造等の加工が極めて難しいという問題があ
った。一般に、このような難加工性材料を加工する方法
として金属容器に包んで（キャニング法）圧延するとい
う方法がある。しかし、この方法を使用して金属ルテニ
ウムのインゴットを例えば圧延する場合には、金属ルテ
ニウムインゴットを他の金属薄板や箔等で包む工程もさ
ることながら、圧延後それを除去する作業を必要とする
など、工程が極めて煩雑となり、またこれによって歩留
りも低下し、著しくコスト高となる欠点があった。した
がって、従来鍛造や圧延でルテニウムターゲットを試験
的に製作することがあっても、実製造上では使用に耐え
ないものであった。[0003] As described above, it is necessary to further improve the purity of a commercially available 3N-level ruthenium powder and process the powder into a sputtering target. However, the melting and casting of metal ruthenium (ingot), whose purity is increased by volatilizing impurities by low melting ruthenium powder by arc melting etc., is hard and brittle, and it is extremely difficult to process such as normal rolling and forging. there were. Generally, as a method of processing such a difficult-to-process material, there is a method of rolling in a metal container (canning method). However, in the case of rolling a metal ruthenium ingot using this method, for example, in addition to the step of wrapping the metal ruthenium ingot with other thin metal sheets or foils, it is necessary to remove the post-rolling work. For example, the steps are extremely complicated, and the yield is reduced, resulting in a significant increase in cost. Therefore, even if a ruthenium target is conventionally produced on a trial basis by forging or rolling, it cannot be used in actual production.
【０００４】このようなことから、従来高純度ルテニウ
ムスパッタリングターゲットを製造する場合には、粉末
冶金法が使用されている。例えば、低い純度のルテニウ
ム粉末を一旦電子ビーム（ＥＢ）溶解して精製し、これ
に塩素ガスを接触させて塩化ルテニウムとした後、これ
をさらに水素還元して高純度化した粉末を得、これをさ
らに焼結してスパッタリングターゲットとする方法があ
る（特開平９−２２７９６５、特開平９−２２７９６６
参照）。しかし、このような焼結による方法は精製工程
数が多く、また最終的に得られたターゲットには焼結体
に特有の空孔が存在し、またこれによってガス等の吸着
が増加するという問題がある。したがって、スパッタリ
ングターゲットとして溶解鍛造品（理論的に相対密度１
００％）に比べ特性に劣ることは否めず、またコスト高
となる欠点を有している。[0004] For this reason, powder metallurgy has conventionally been used for producing a high-purity ruthenium sputtering target. For example, low purity ruthenium powder is once purified by dissolving it with an electron beam (EB), and then contacted with chlorine gas to form ruthenium chloride, which is further reduced with hydrogen to obtain a highly purified powder. Are further sintered to obtain a sputtering target (JP-A-9-227965, JP-A-9-227966).
reference). However, such a sintering method has many purification steps, and the final target has pores peculiar to the sintered body, which increases the adsorption of gas and the like. There is. Therefore, a melt-forged product (theoretically, a relative density of 1
(00%), it is inevitable that the characteristics are inferior, and the cost is high.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、上記の問題
を解決するために、５Ｎ（９９．９９９ｗｔ％）レベル
以上の均一な鍛造組織を有する高純度ルテニウムスパッ
タリングターゲットを得、さらに３Ｎ（９９．９ｗｔ
％）レベルの比較的低純度のルテニウム粉末を使用して
５レベル以上の均一な鍛造組織を有する高純度ルテニウ
ムスパッタリングターゲットを簡便にかつ安定して製造
する方法を得ることを課題とする。SUMMARY OF THE INVENTION In order to solve the above-mentioned problems, the present invention provides a high-purity ruthenium sputtering target having a uniform forged structure of 5N (99.999 wt%) or more, and further obtains a 3N (99%). .9wt
It is an object of the present invention to provide a method for easily and stably producing a high-purity ruthenium sputtering target having a uniform forging structure of 5 or more levels using ruthenium powder having a relatively low purity of (%) level.
【０００６】[0006]
【課題を解決するための手段】本発明は、 １．酸素１０ｗｔｐｐｍ以下、窒素１０ｗｔｐｐｍ以下
であり、鍛造組織を備えていることを特徴とする高純度
ルテニウムターゲット。 ２．平均結晶粒度が５ｍｍ以下であることを特徴とする
上記１記載の高純度ルテニウムターゲット。 ３．５Ｎレベル以上の純度を有することを特徴とする上
記１又は２記載の高純度ルテニウムターゲット。 ４．ルテニウム粉末をＥＢ溶解により高純度化し、次に
これを凝固させてインゴットを形成し、さらに該インゴ
ットを１４００〜２０００°Ｃで鍛造することを特徴と
する高純度ルテニウムターゲットの製造方法。 ５．３Ｎレベルのルテニウム粉末をアルゴン又は水素ガ
ス雰囲気中、８００〜１６００°Ｃで焼結した後、ＥＢ
溶解することを特徴とする上記４記載の高純度ルテニウ
ムターゲットの製造方法。 ６．酸素１０ｗｔｐｐｍ以下、窒素１０ｗｔｐｐｍ以下
であることを特徴とする上記４又は５に記載の高純度ル
テニウムターゲットの製造方法。 ７．平均結晶粒度が５ｍｍ以下であることを特徴とする
上記４〜６のそれぞれに記載の高純度ルテニウムターゲ
ットの製造方法。 ８．５Ｎレベル以上の純度を有することを特徴とする上
記４〜７のそれぞれに記載の高純度ルテニウムターゲッ
トの製造方法。 ９．２回以上のＥＢ溶解を行うことを特徴とする上記４
〜８のそれぞれに記載の高純度ルテニウムターゲットの
製造方法。 を提供する。The present invention provides: A high-purity ruthenium target containing 10 wtppm or less of oxygen and 10 wtppm or less of nitrogen and having a forged structure. 2. 2. The high-purity ruthenium target according to the above 1, wherein the average crystal grain size is 5 mm or less. 3. The high-purity ruthenium target according to the above 1 or 2, wherein the target has a purity of 3.5N level or more. 4. A method for producing a high-purity ruthenium target, comprising purifying ruthenium powder by EB melting, solidifying the same, forming an ingot, and forging the ingot at 1400 to 2000 ° C. After sintering ruthenium powder of 5.3N level in an argon or hydrogen gas atmosphere at 800 to 1600 ° C, EB
5. The method for producing a high-purity ruthenium target according to the above item 4, wherein the target is dissolved. 6. 6. The method for producing a high-purity ruthenium target according to 4 or 5 above, wherein oxygen is 10 wtppm or less and nitrogen is 10 wtppm or less. 7. 7. The method for producing a high-purity ruthenium target according to any one of the above items 4 to 6, wherein the average crystal grain size is 5 mm or less. 8. The method for producing a high-purity ruthenium target according to any one of the above items 4 to 7, wherein the method has a purity of 8.5N level or more. 9. The above-mentioned item 4 wherein EB dissolution is performed twice or more.
9. The method for producing a high-purity ruthenium target according to any one of Items 1 to 8. I will provide a.
【０００７】[0007]
【発明の実施の形態】本発明の高純度ルテニウムターゲ
ットは、酸素１０ｗｔｐｐｍ以下、窒素１０ｗｔｐｐｍ
以下であり、鍛造組織を備えている。また、該ターゲッ
トは好適には５ｍｍ以下の平均結晶粒度を有しており、
５Ｎレベル以上の純度を有する高純度ルテニウムスパッ
タリングターゲットである。ルテニウムターゲットの酸
素１０ｗｔｐｐｍ以下、窒素１０ｗｔｐｐｍ以下である
ことはスパッタリングの際のパーティクル発生が少ない
という点で極めて優れたものである。また、５Ｎレベル
以上の純度を有する高純度ルテニウムスパッタリングタ
ーゲットは半導体特性が良いという点で優れている。本
発明の高純度ルテニウムスパッタリングターゲット製造
に際しては、３Ｎレベルのルテニウム粉末を使用するこ
とができ、このルテニウム粉末をＥＢ溶解して不純物を
揮発又はスラグとして除去することにより高純度化し、
さらにこれを凝固させてインゴットを製造する。DESCRIPTION OF THE PREFERRED EMBODIMENTS The high-purity ruthenium target of the present invention has an oxygen content of 10 wt ppm or less and a nitrogen content of 10 wt ppm.
The following is provided with a forging structure. In addition, the target preferably has an average grain size of 5 mm or less,
It is a high-purity ruthenium sputtering target having a purity of 5N level or more. The fact that the oxygen content of the ruthenium target is 10 wtppm or less and the nitrogen content is 10 wtppm or less is extremely excellent in that particles are less generated during sputtering. Further, a high-purity ruthenium sputtering target having a purity of 5N level or more is excellent in that semiconductor characteristics are good. In producing the high-purity ruthenium sputtering target of the present invention, a 3N-level ruthenium powder can be used, and the ruthenium powder is highly purified by dissolving the ruthenium powder by EB and removing impurities as volatile or slag,
This is further solidified to produce an ingot.
【０００８】ＥＢ溶解に際しては、前記３Ｎレベルのル
テニウム粉末を予めＰＶＡ（ポリビニルアルコール）等
を混ぜて固め、アルゴン又は水素ガス（非酸素、非窒
素）雰囲気中、８００〜１６００°Ｃで焼結し焼結体と
した後、ＥＢ溶解することが望ましい。焼結温度８００
〜１６００°Ｃの範囲で焼結するのは、ＥＢ溶解時にス
プラッシュの発生が少なくすることができるという理由
による。なお、ＥＢ溶解２回以上行うことが望ましい。
１回のＥＢ溶解では内部に巣が多く発生し易く、品質低
下や歩留り低下となり易いからである。このＥＢ溶解に
よりルテニウムに存在する不純物の揮発成分は除去さ
れ、またスラグとして除去できる。 これによって、５
Ｎレベルの高純度ルテニウムインゴットを市販の３Ｎレ
ベルのルテニウム粉末から容易に得ることができる。特
に、酸素１０ｗｔｐｐｍ以下、窒素１０ｗｔｐｐｍ以下
とすることができる。ＥＢ溶解前の市販の３Ｎレベルの
ルテニウム粉末の不純物濃度を表１に示す。なお、表１
の濃度はｗｔｐｐｍである。In dissolving the EB, the 3N-level ruthenium powder is previously mixed with PVA (polyvinyl alcohol) or the like, solidified, and sintered at 800 to 1600 ° C. in an argon or hydrogen gas (non-oxygen, non-nitrogen) atmosphere. After forming the sintered body, it is desirable to dissolve the EB. Sintering temperature 800
The reason for sintering in the range of １1600 ° C. is that the generation of splash during EB melting can be reduced. In addition, it is desirable to perform EB dissolution twice or more.
This is because a single EB dissolution easily causes many nests inside, which tends to lower the quality and yield. By this EB dissolution, volatile components of impurities present in ruthenium are removed and can be removed as slag. This gives 5
An N-level high-purity ruthenium ingot can be easily obtained from a commercially available 3N-level ruthenium powder. In particular, oxygen can be 10 wtppm or less and nitrogen can be 10 wtppm or less. Table 1 shows the impurity concentration of a commercially available 3N-level ruthenium powder before EB dissolution. Table 1
Is wtppm.
【０００９】[0009]
【表１】 [Table 1]
【００１０】次に、このようにして得た５Ｎレベルの高
純度ルテニウムインゴットを１４００〜２０００°Ｃの
範囲で鍛造する。１４００°Ｃ未満では鍛造により割れ
が入り、また２０００°Ｃを超える温度ではエネルギー
コストが増大し、好ましくないからである。また、鍛造
中に温度低下するとターゲット材に割れが発生するの
で、恒温鍛造が望ましい。上記温度範囲において、割れ
の発生の無い鍛造品が得られる。鍛造によりほぼターゲ
ットに近い形にまで加工するが、さらに旋盤等で表面を
加工しかつ仕上げ加工してターゲットに仕上げる。これ
によって、粉末焼結品に比べ、はるかに成分が均一で、
高密度、高純度の高純度ルテニウムスパッタリングター
ゲットを低コストで得ることができる。Next, the 5N level high purity ruthenium ingot thus obtained is forged in a range of 1400 to 2000 ° C. If the temperature is lower than 1400 ° C., cracking is caused by forging, and if the temperature exceeds 2000 ° C., energy cost increases, which is not preferable. Further, if the temperature is lowered during forging, a crack occurs in the target material, so that constant temperature forging is desirable. Within the above temperature range, a forged product free from cracks can be obtained. It is processed by forging to a shape almost similar to the target, but the surface is further processed with a lathe or the like and finish processing is performed to finish the target. As a result, the components are much more uniform than powder sintered products,
A high-purity, high-purity ruthenium sputtering target with high purity can be obtained at low cost.
【００１１】[0011]
【実施例】次に、実施例について説明する。なお、本実
施例は発明の一例を示すためのものであり、本発明はこ
れらの実施例に制限されるものではない。すなわち、本
発明の技術思想に含まれる他の態様及び変形を含むもの
である。Next, an embodiment will be described. It should be noted that the present embodiment is merely an example of the present invention, and the present invention is not limited to these embodiments. That is, it includes other aspects and modifications included in the technical idea of the present invention.
【００１２】（実施例１）前記表１で示した不純物濃度
を有する市販の３Ｎレベルのルテニウム粉末約１０ｋｇ
に、予めＰＶＡ（ポリビニルアルコール）を混ぜて固
め、アルゴンガス雰囲気中、１０００°Ｃで焼結し焼結
体とした。次に、これを３回のＥＢ溶解を実施し９．４
ｋｇのインゴットを得た。この溶解により巣の発生は小
さかった。このインゴットをさらに、１６００°Ｃの条
件で鍛造し、φ３５０×８ｍｍｔの板を得た。これを旋
盤加工し高純度ルテニウムスパッタリングターゲットを
得た。このようにして得たターゲットの不純物濃度を表
２に示す。なお、表２の濃度はｗｔｐｐｍである。平均
粒径は約３ｍｍであった。(Example 1) Approximately 10 kg of a commercially available 3N-level ruthenium powder having the impurity concentration shown in Table 1 above
Was mixed with PVA (polyvinyl alcohol) in advance and solidified, and sintered at 1000 ° C. in an argon gas atmosphere to obtain a sintered body. Next, this was subjected to EB dissolution three times, and 9.4 was performed.
kg ingot was obtained. The nest was small due to this dissolution. The ingot was further forged at 1600 ° C. to obtain a plate of φ350 × 8 mmt. This was turned into a high-purity ruthenium sputtering target. Table 2 shows the impurity concentrations of the target thus obtained. The concentrations in Table 2 are wtppm. The average particle size was about 3 mm.
【００１３】[0013]
【表２】 [Table 2]
【００１４】表２に示す通り、酸素及び窒素の含有量は
それぞれ１０ｗｔｐｐｍ未満であり、５Ｎレベルの高純
度のルテニウムスパッタリングターゲットを得ることが
できた。本発明は従来の焼結品に比べ工程数が少なく、
高純度、高密度のターゲットを低コストで製造すること
ができる。As shown in Table 2, the contents of oxygen and nitrogen were each less than 10 wtppm, and a 5N-level high-purity ruthenium sputtering target could be obtained. The present invention has fewer steps compared to conventional sintered products,
High-purity, high-density targets can be manufactured at low cost.
【００１５】（実施例２）前記表１で示した不純物濃度
を有する市販の３Ｎレベルのルテニウム粉末約１０ｋｇ
に、予めＰＶＡ（ポリビニルアルコール）を混ぜて固
め、アルゴンガス雰囲気中、１４００°Ｃで焼結し焼結
体とした。次に、これを２回のＥＢ溶解を実施し９．４
ｋｇのインゴットを得た。この溶解により巣の発生は小
さかった。このインゴットをさらに、１５００°Ｃの条
件で鍛造し、φ３５０×８ｍｍｔの板を得た。これを旋
盤加工し高純度ルテニウムスパッタリングターゲットを
得た。このようにして得たターゲットの純度は実施例１
と同程度であった。また、平均粒径は約２．５ｍｍであ
った。Example 2 Approximately 10 kg of a commercially available 3N-level ruthenium powder having the impurity concentration shown in Table 1 above
Was mixed with PVA (polyvinyl alcohol) in advance and solidified, and sintered at 1400 ° C. in an argon gas atmosphere to obtain a sintered body. Next, this was subjected to EB dissolution twice and 9.4 times.
kg ingot was obtained. The nest was small due to this dissolution. The ingot was further forged under the condition of 1500 ° C. to obtain a φ350 × 8 mmt plate. This was turned into a high-purity ruthenium sputtering target. The purity of the target thus obtained was determined in Example 1.
Was about the same. The average particle size was about 2.5 mm.
【００１６】（実施例３）前記表１で示した不純物濃度
を有する市販の３Ｎレベルのルテニウム粉末約１０ｋｇ
に、予めＰＶＡ（ポリビニルアルコール）を混ぜて固
め、アルゴンガス雰囲気中、８００°Ｃで焼結し焼結体
とした。次に、これを４回のＥＢ溶解を実施し９．４ｋ
ｇのインゴットを得た。この溶解により巣の発生は小さ
かった。このインゴットをさらに、１８００°Ｃの条件
で鍛造し、φ３５０×８ｍｍｔの板を得た。これを旋盤
加工し高純度ルテニウムスパッタリングターゲットを得
た。このようにして得たターゲットの純度は実施例１と
同程度であった。また、平均粒径は約４ｍｍであった。Example 3 Approximately 10 kg of a commercially available 3N-level ruthenium powder having the impurity concentration shown in Table 1 above
Was mixed with PVA (polyvinyl alcohol) in advance and solidified, and sintered at 800 ° C. in an argon gas atmosphere to obtain a sintered body. Next, this was subjected to EB dissolution four times to obtain 9.4k.
g of ingot was obtained. The nest was small due to this dissolution. This ingot was further forged under the conditions of 1800 ° C. to obtain a φ350 × 8 mmt plate. This was turned into a high-purity ruthenium sputtering target. The purity of the target thus obtained was about the same as in Example 1. The average particle size was about 4 mm.
【００１７】（比較例１）ＥＢ溶解を１回実施した以外
は、実施例１と同一の材料を使用し、同様の条件でイン
ゴットを得た。しかし、ＥＢ溶解が十分でないためにイ
ンゴット内に巣が多く、この巣が発生した多くの部分を
インゴットから削除する必要があるため、歩留りが悪く
なり、ターゲットの作製には使用できなかった。(Comparative Example 1) An ingot was obtained under the same conditions as in Example 1 except that the EB melting was performed once. However, since EBs are not sufficiently dissolved, there are many nests in the ingot, and it is necessary to delete many portions where the nests have occurred from the ingot.
【００１８】（比較例２）実施例１と同一の材料を使用
し、ＥＢ溶解を３回実施し他は同様の条件でインゴット
を得た。そして１３００°Ｃで鍛造した。しかし、鍛造
温度が低いためにインゴットの加工が難しく、割れが発
生した。このためターゲットへの加工は中断した。(Comparative Example 2) Using the same material as in Example 1, EB melting was performed three times, and an ingot was obtained under the same conditions except for the above. And it forged at 1300 ° C. However, processing of the ingot was difficult due to the low forging temperature, and cracks occurred. For this reason, processing on the target was suspended.
【００１９】[0019]
【発明の効果】本発明は、従来の金属容器に包んで（キ
ャニング法）圧延するなどの複雑及びコスト増となる手
法をとる必要がなく、また粉末冶金特有の空孔の発生
（密度低下）することなく、焼結品に比べ工程数が少な
く、高純度、高密度のルテニウムスパッタリングターゲ
ットを安価に得ることができるという優れた効果を有す
る。According to the present invention, it is not necessary to take a complicated and cost-increasing method such as rolling in a conventional metal container (canning method), and generation of voids (density reduction) peculiar to powder metallurgy. Therefore, there is an excellent effect that the number of steps is smaller than that of a sintered product, and a high-purity, high-density ruthenium sputtering target can be obtained at low cost.
Claims (9)
ｐｐｍ以下であり、鍛造組織を備えていることを特徴と
する高純度ルテニウムターゲット。Claims: 1. Oxygen 10 wtppm or less, nitrogen 10 wtppm
A high-purity ruthenium target which is at most ppm and has a forged structure.
特徴とする請求項１記載の高純度ルテニウムターゲッ
ト。2. The high-purity ruthenium target according to claim 1, wherein the average crystal grain size is 5 mm or less.
徴とする請求項１又は２記載の高純度ルテニウムターゲ
ット。3. The high-purity ruthenium target according to claim 1, wherein the target has a purity of 5N level or more.
化し、次にこれを凝固させてインゴットを形成し、さら
に該インゴットを１４００〜２０００°Ｃで鍛造するこ
とを特徴とする高純度ルテニウムターゲットの製造方
法。4. The production of a high-purity ruthenium target, characterized in that the ruthenium powder is highly purified by EB melting, then solidified to form an ingot, and the ingot is forged at 1400 to 2000 ° C. Method.
又は水素ガス雰囲気中、８００〜１６００°Ｃで焼結し
た後、ＥＢ溶解することを特徴とする請求項４記載の高
純度ルテニウムターゲットの製造方法。5. The method for producing a high-purity ruthenium target according to claim 4, wherein the 3N-level ruthenium powder is sintered at 800 to 1600 ° C. in an argon or hydrogen gas atmosphere and then EB-dissolved.
ｐｐｍ以下であることを特徴とする請求項４又は５に記
載の高純度ルテニウムターゲットの製造方法。6. Oxygen 10 wtppm or less, nitrogen 10 wtppm
The method for producing a high-purity ruthenium target according to claim 4, wherein the concentration is at most ppm.
特徴とする請求項４〜６のそれぞれに記載の高純度ルテ
ニウムターゲットの製造方法。7. The method for producing a high-purity ruthenium target according to claim 4, wherein the average crystal grain size is 5 mm or less.
徴とする請求項４〜７のそれぞれに記載の高純度ルテニ
ウムターゲットの製造方法。8. The method for producing a high-purity ruthenium target according to claim 4, wherein the target has a purity of 5N level or more.
する請求項４〜８のそれぞれに記載の高純度ルテニウム
ターゲットの製造方法。9. The method for producing a high-purity ruthenium target according to claim 4, wherein EB melting is performed twice or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001131378A JP3878432B2 (en) | 2001-04-27 | 2001-04-27 | High-purity ruthenium target and method for producing the target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001131378A JP3878432B2 (en) | 2001-04-27 | 2001-04-27 | High-purity ruthenium target and method for producing the target |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002327265A true JP2002327265A (en) | 2002-11-15 |
| JP3878432B2 JP3878432B2 (en) | 2007-02-07 |
Family
ID=18979578
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001131378A Expired - Lifetime JP3878432B2 (en) | 2001-04-27 | 2001-04-27 | High-purity ruthenium target and method for producing the target |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3878432B2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1724364A1 (en) * | 2004-03-01 | 2006-11-22 | Nippon Mining & Metals Co., Ltd. | HIGH-PURITY Ru POWDER, SPUTTERING TARGET OBTAINED BY SINTERING THE SAME, THIN FILM OBTAINED BY SPUTTERING THE TARGET AND PROCESS FOR PRODUCING HIGH-PURITY RU POWDER |
| EP2055793A1 (en) * | 2007-10-29 | 2009-05-06 | Heraeus, Inc. | Methodology for recycling RU and RU-alloy deposition targets & targets made of recycled RU and RU-based alloy powders |
| JP4800317B2 (en) * | 2005-10-14 | 2011-10-26 | Ｊｘ日鉱日石金属株式会社 | High purity Ru alloy target, method for producing the same, and sputtered film |
| KR20140128356A (en) | 2012-07-30 | 2014-11-05 | 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 | Ruthenium sputtering target and ruthenium alloy sputtering target |
-
2001
- 2001-04-27 JP JP2001131378A patent/JP3878432B2/en not_active Expired - Lifetime
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1724364A1 (en) * | 2004-03-01 | 2006-11-22 | Nippon Mining & Metals Co., Ltd. | HIGH-PURITY Ru POWDER, SPUTTERING TARGET OBTAINED BY SINTERING THE SAME, THIN FILM OBTAINED BY SPUTTERING THE TARGET AND PROCESS FOR PRODUCING HIGH-PURITY RU POWDER |
| JPWO2005083136A1 (en) * | 2004-03-01 | 2008-04-24 | 日鉱金属株式会社 | High purity Ru powder, sputtering target obtained by sintering the high purity Ru powder, thin film obtained by sputtering the target, and method for producing high purity Ru powder |
| EP1724364A4 (en) * | 2004-03-01 | 2009-11-04 | Nippon Mining Co | HIGH-PURITY Ru POWDER, SPUTTERING TARGET OBTAINED BY SINTERING THE SAME, THIN FILM OBTAINED BY SPUTTERING THE TARGET AND PROCESS FOR PRODUCING HIGH-PURITY RU POWDER |
| JP2010047844A (en) * | 2004-03-01 | 2010-03-04 | Nippon Mining & Metals Co Ltd | HIGH-PURITY Ru POWDER, SPUTTERING TARGET OBTAINED BY SINTERING THE HIGH-PURITY Ru POWDER, THIN FILM OBTAINED BY SPUTTERING THE TARGET, AND METHOD FOR PREPARING HIGH-PURITY Ru POWDER |
| JP4522991B2 (en) * | 2004-03-01 | 2010-08-11 | 日鉱金属株式会社 | Method for producing high purity Ru powder |
| JP4800317B2 (en) * | 2005-10-14 | 2011-10-26 | Ｊｘ日鉱日石金属株式会社 | High purity Ru alloy target, method for producing the same, and sputtered film |
| EP2055793A1 (en) * | 2007-10-29 | 2009-05-06 | Heraeus, Inc. | Methodology for recycling RU and RU-alloy deposition targets & targets made of recycled RU and RU-based alloy powders |
| JP2009108400A (en) * | 2007-10-29 | 2009-05-21 | Heraeus Inc | METHODOLOGY FOR RECYCLING RUTHENIUM (Ru) AND RUTHENIUM (Ru) ALLOY DEPOSITION TARGET AND TARGET MADE OF RECYCLED RUTHENIUM (Ru) AND RUTHENIUM (Ru)-BASED ALLOY POWDER |
| US8118906B2 (en) | 2007-10-29 | 2012-02-21 | Heraeus Inc. | Methodology for recycling Ru and Ru-alloy deposition targets and targets made of recycled Ru and Ru-based alloy powders |
| KR20140128356A (en) | 2012-07-30 | 2014-11-05 | 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 | Ruthenium sputtering target and ruthenium alloy sputtering target |
| US10319571B2 (en) | 2012-07-30 | 2019-06-11 | Jx Nippon Mining & Metals Corporation | Ruthenium sputtering target and ruthenium alloy sputtering target |
| US10943773B2 (en) | 2012-07-30 | 2021-03-09 | Jx Nippon Mining & Metals Corporation | Ruthenium sputtering target and ruthenium alloy sputtering target |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3878432B2 (en) | 2007-02-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5113134B2 (en) | Method for producing Ni-Pt alloy and method for producing the same alloy target | |
| JP6077102B2 (en) | Titanium target for sputtering and manufacturing method thereof | |
| TWI519660B (en) | Sputtering titanium target | |
| JP2004162117A (en) | Ta SPUTTERING TARGET AND ITS PRODUCTION METHOD | |
| JP3782353B2 (en) | Titanium target for sputtering | |
| TW201533248A (en) | High-purity tantalum powder and preparation method therefor | |
| KR20200037461A (en) | Method for producing sputtering target, and sputtering target | |
| KR101469873B1 (en) | Manufacturing method of a high purity and refining Ru alloy powder | |
| US20150232980A1 (en) | Cu-Ga Alloy Sputtering Target, and Method for Producing Same | |
| JP5144576B2 (en) | Titanium target for sputtering | |
| JP2002327265A (en) | High purity ruthenium target and manufacturing method therefor | |
| JP2015196885A (en) | Manufacturing method of ultra-low oxygen/ultra-high pure chromium target and ultra-low oxygen/ultra-high pure chromium target | |
| JP3792535B2 (en) | Manufacturing method of high purity ruthenium target | |
| JP3998972B2 (en) | Method for producing sputtering tungsten target | |
| JPH0941131A (en) | Production of high purity iridium or ruthenium sputtering target | |
| JPH06264233A (en) | Sputtering target for producing tft | |
| KR20170045273A (en) | Cast titanium slab for use in hot rolling and unlikely to exhibit surface defects, and method for producing same | |
| JPH11158565A (en) | Production of titanium ingot | |
| KR20140115953A (en) | Cu-ga alloy sputtering target, molten product for the sputtering target, and method of producing same | |
| JPH04116161A (en) | Titanium target material and production thereof | |
| JP2012087373A (en) | Method for storing high purity sponge-titanium particle, and method for producing high purity titanium ingot using the same | |
| JPH0995743A (en) | Production of smelted metallic material, smelted metallic material and electron beam melting equipment | |
| JPH1161392A (en) | Production of sputtering target for forming ru thin film | |
| JPH0813141A (en) | Sputtering target and its production | |
| JP2004137580A (en) | Method for producing iridium sputtering target, and target obtained by the method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20060807 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20060815 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20060928 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20061031 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20061102 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 Ref document number: 3878432 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091110 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101110 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101110 Year of fee payment: 4 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313111 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101110 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20111110 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20111110 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121110 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121110 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131110 Year of fee payment: 7 |
|
| S531 | Written request for registration of change of domicile |
Free format text: JAPANESE INTERMEDIATE CODE: R313531 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| EXPY | Cancellation because of completion of term |