JP2757287B2 - Manufacturing method of tungsten target - Google Patents
Manufacturing method of tungsten targetInfo
- Publication number
- JP2757287B2 JP2757287B2 JP1286699A JP28669989A JP2757287B2 JP 2757287 B2 JP2757287 B2 JP 2757287B2 JP 1286699 A JP1286699 A JP 1286699A JP 28669989 A JP28669989 A JP 28669989A JP 2757287 B2 JP2757287 B2 JP 2757287B2
- Authority
- JP
- Japan
- Prior art keywords
- density
- hip
- target
- sintered body
- tungsten
- 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.)
- Expired - Lifetime
Links
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims description 14
- 229910052721 tungsten Inorganic materials 0.000 title claims description 11
- 239000010937 tungsten Substances 0.000 title claims description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000000034 method Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 5
- 238000001513 hot isostatic pressing Methods 0.000 description 20
- 239000002245 particle Substances 0.000 description 12
- 238000004544 sputter deposition Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 235000012431 wafers Nutrition 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
- Powder Metallurgy (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、半導体デバイスに使用される電極、配線材
料形成に用いられる高純度タングステンターゲットに関
するものである。Description: TECHNICAL FIELD The present invention relates to a high-purity tungsten target used for forming electrodes and wiring materials used in semiconductor devices.
近年の超LSIの高集積化に伴い、配線幅の減少、配線
長の増大により、配線材料の抵抗による信号遅延が問題
となり、より抵抗値の低い材料が要求されている。With the recent increase in the integration of VLSIs, a reduction in the wiring width and an increase in the wiring length have caused a problem of signal delay due to the resistance of the wiring material.
ゲート電極材としては、抵抗値の低いタングステン、
モリブデンなどの高融点金属が有望である。As the gate electrode material, tungsten having a low resistance value,
Refractory metals such as molybdenum are promising.
タングステン、モリブデン膜の形成法としては、スパ
ッタ法およびCVD法があるが、成膜の生産性および安定
性の面でスパッタ法が有利である。As a method for forming a tungsten or molybdenum film, there are a sputtering method and a CVD method, and the sputtering method is advantageous in terms of productivity and stability of film formation.
スパッタ法で使用されるタングステンおよびモリブデ
ンスパッタリングターゲットの製造方法としては、電子
ビーム溶解などを利用した溶解法（特開昭60−66425
号、特開昭61−107728号）とホットプレスなどを利用し
た粉末−焼結法がある。As a method for producing a tungsten and molybdenum sputtering target used in the sputtering method, a melting method utilizing electron beam melting or the like (Japanese Patent Laid-Open No. 60-66425).
And a powder-sintering method utilizing hot pressing or the like.
しかし、溶解法で作製したインゴットは、タングステ
ンが高融点（W:3422℃）でかつ高純度であるため、結晶
粒は粗大化する。結晶粒が粗大化すると、その後の機械
加工時に容易に割れてしまう。また、結晶粒粗大化のタ
ーゲットを用いてスパッタリングを実施した場合、結晶
粒の異方性のため均一な膜が形成されない。However, in the ingot produced by the melting method, the crystal grains become coarse because tungsten has a high melting point (W: 3422 ° C.) and high purity. When the crystal grains become coarse, they are easily broken during subsequent machining. Further, when sputtering is performed using a target for coarsening crystal grains, a uniform film cannot be formed due to anisotropy of crystal grains.
この結晶粒粗大化を添加物により、防止する方法が提
案（特開昭61−116835号参照）されているが、添加物が
膜特性を劣化する場合がある。Although a method of preventing the coarsening of the crystal grains with an additive has been proposed (see Japanese Patent Application Laid-Open No. 61-116835), the additive may deteriorate the film characteristics.
一方、粉末−焼結法で作製したターゲットは、結晶粒
は微細であるが、タングステンが高融点材料であるた
め、高密度を得ることが極めて困難である。On the other hand, although the target manufactured by the powder-sintering method has fine crystal grains, it is extremely difficult to obtain a high density because tungsten is a high melting point material.
例えば、比較的高融点（1905℃）の高Cr合金材の高密
度化手法として特公昭60−58289号に開示されたもので
ある。特公昭60−58289号によると、原料粉末に吸着し
ているガス、水分を除去してから特定条件下で加圧焼結
することによりほぼ真密度の焼結体が得られているとし
ているが、ＷはCrより高融点であり、特公昭60−58289
号に開示される焼結温度等の条件では、高密度化が困難
であり、本発明者の検討によると、ホットプレスまたは
HIP（熱間静水圧プレス）処理では相対密度85％程度が
限度である。For example, Japanese Patent Publication No. 60-58289 discloses a method for increasing the density of a high Cr alloy material having a relatively high melting point (1905 ° C.). According to Japanese Examined Patent Publication No. 60-58289, a sintered compact of almost true density is obtained by pressure sintering under specific conditions after removing the gas and moisture adsorbed on the raw material powder. , W has a higher melting point than Cr.
Under the conditions such as the sintering temperature disclosed in No. 5, it is difficult to increase the density, and according to the study of the present inventors, hot pressing or
In the HIP (hot isostatic pressing) process, the relative density is limited to about 85%.
処理条件を過酷（例えば保持温度1500℃以上で2000at
mの高圧）にしてやれば、高密度が得られる可能性があ
るが、設備的なことを考慮すると非現実的である。密度
の低いターゲットを用いてスパッタリングを実施した場
合、スパッタ時に割れる可能性が大きい。また、生成さ
れた膜中のパーティクル（異物）数が著しく多くなり、
ウェハーの歩留低下の原因となる。Severe processing conditions (for example, 2000at at holding temperature of 1500 ℃ or more)
(high pressure of m), there is a possibility that a high density can be obtained, but it is impractical considering equipment. When sputtering is performed using a low-density target, the possibility of cracking during sputtering is high. In addition, the number of particles (foreign matter) in the generated film significantly increases,
This causes a reduction in the yield of the wafer.
本発明は、以上の状況に鑑み、微細組織であり、かつ
高密度を有するタングステンターゲットの製造方法の提
供を課題とする。In view of the above circumstances, an object of the present invention is to provide a method for manufacturing a tungsten target having a fine structure and a high density.
本発明者は、前記目的を達成すべく種々検討した結
果、Ｗからなる予備焼結体を得たのち、熱間塑性加工を
施すことにより、微細組織を有し、かつ相対密度が99％
以上の高密度の焼結体ターゲットを得ることができるこ
とを知見し、本発明を完成するに至った。The present inventor has conducted various studies to achieve the above object. As a result, after obtaining a pre-sintered body made of W, the pre-sintered body is subjected to hot plastic working to have a fine structure and a relative density of 99%.
The inventor has found that a high-density sintered body target as described above can be obtained, and has completed the present invention.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
本発明において、まずＷの原料粉末が準備される。 In the present invention, first, a raw material powder of W is prepared.
この原料粉末は、ターゲットとして高純度が要求され
るので、高純度であることが望ましく、特に99.999％以
上の純度であることが望ましい。また、粉末の粒度は、
FSSS（フィッシャー粒度）で５μｍ以下であることが望
ましい。Since the raw material powder is required to have high purity as a target, it is desirable that the raw material powder has high purity, particularly 99.999% or more. The particle size of the powder is
The FSSS (Fisher particle size) is desirably 5 μm or less.
次いで、以上の粉末を用い、予備焼結体を製造する。 Next, a preliminary sintered body is manufactured using the above powder.
ここで焼結方法としては、通常の焼結の他、HIP、ホ
ットプレス等の公知の焼結手段を採用することができ
る。Here, as the sintering method, besides ordinary sintering, known sintering means such as HIP and hot pressing can be adopted.
次いで実施される熱間塑性加工の工程簡略化のために
は、予備焼結体の密度が高いことが望ましく、この場
合、焼結方法としてHIPまたはホットプレスが望まし
い。In order to simplify the subsequent hot plastic working process, the density of the pre-sintered body is desirably high. In this case, HIP or hot pressing is desirable as the sintering method.
HIPを適用する場合は、圧密用封入缶（以下HIP缶とい
う）に粉末を充填し、10-5torr以上の真空下で200℃以
上に加熱し、粉末に吸着したガス、水分を除去すること
が要求される。ガス、水分が存在すると焼結性の低下を
まねくためである。この操作終了後、HIP缶は封止さ
れ、HIPに供される。When applying HIP, fill the compacting can (hereinafter referred to as HIP can) with powder and heat it to 200 ° C or more under a vacuum of 10 -5 torr or more to remove gas and moisture adsorbed on the powder. Is required. This is because the presence of gas and moisture may cause a decrease in sinterability. After this operation, the HIP can is sealed and subjected to HIP.
HIP条件としては、HIP温度1150〜1350℃、HIP圧力100
0atm以上が望ましい。As HIP conditions, HIP temperature 1150-1350 ° C, HIP pressure 100
0 atm or more is desirable.
HIP温度を1150℃以上とするのは、この温度未満では
密度向上が十分に達成されず、また1350℃以下とするの
は、1350℃を越えると組織が粗大化するためである。The reason why the HIP temperature is set to 1150 ° C. or higher is that if the temperature is lower than this temperature, the density cannot be sufficiently improved, and the temperature is set to 1350 ° C. or lower because if it exceeds 1350 ° C., the structure becomes coarse.
また、HIP圧力を1000atm以上とするのは、1000atm未
満では十分な密度向上を達成することが困難だからであ
る。In addition, the reason why the HIP pressure is set to 1000 atm or more is that it is difficult to achieve a sufficient density improvement when the HIP pressure is less than 1000 atm.
以上の条件によれば、相対密度85％程度に圧密化され
た予備焼結体を得ることができる。According to the above conditions, it is possible to obtain a pre-sintered body compacted to a relative density of about 85%.
得られた予備焼結体に熱間塑性加工を施し、高密度化
を図る。例えば予備焼結体の密度が85％程度の場合に
は、60％程度の加工率を付与することにより、99.9％以
上のほぼ真密度の焼結体が得られる。The obtained pre-sintered body is subjected to hot plastic working to increase the density. For example, when the density of the pre-sintered body is about 85%, a substantially true density sintered body of 99.9% or more can be obtained by giving a processing rate of about 60%.
加工温度は、1200〜1500℃の範囲が望ましい。1200℃
未満では、密度向上が十分に達成されず、また1500℃を
越えると組織の粗大化を招くためである。The processing temperature is desirably in the range of 1200 to 1500 ° C. 1200 ℃
If it is less than 1, the density cannot be sufficiently improved, and if it exceeds 1500 ° C., the structure becomes coarse.
なお、熱間加工時の汚染は極力避ける必要があり、HI
Pによる場合は、焼結体が完全にHIP缶内に封入されてい
るため、汚染は皆無であるが、その他の手段による場合
は予備焼結体をHIPと同様に缶内に封入することが望ま
れる。It is necessary to minimize contamination during hot working.
In the case of P, the sintered body is completely sealed in the HIP can, so there is no contamination.However, in the case of other means, the pre-sintered body can be sealed in the can in the same way as HIP. desired.
以上の方法によれば、平均粒径10μｍ以下の微細組織
を有し、かつ相対密度99％以上の高密度のタングステン
ターゲットが得られる。According to the above method, a high-density tungsten target having a fine structure with an average particle size of 10 μm or less and a relative density of 99% or more can be obtained.
高純度タングステン粉末（Ｗ≧99.999％〔放射性元素
含有量3ppb以下、アルカリ金属含有量100ppb以下〕、粒
度FSSS（フィッシャー粒度）で５μｍ以下）を内容積40
0×300×30（mm）の圧密用封入缶（HIP缶）に充填し、
５×10-5Torrに真空排気しながら、400℃×５時間加熱
し、表面吸着ガスおよび水分を放出した。加熱脱気後封
止し、1250℃×２時間、1000atmの条件でHIP処理を行な
った。この時得られた焼結体の密度は相対密度で80〜85
％である。High-purity tungsten powder (W ≧ 99.999% [radioactive element content 3 ppb or less, alkali metal content 100 ppb or less], particle size FSSS (Fisher particle size) 5 μm or less)
Fill into a sealed can (HIP can) of 0 × 300 × 30 (mm),
While evacuating to 5 × 10 −5 Torr, the substrate was heated at 400 ° C. for 5 hours to release the surface adsorbed gas and moisture. After heating and degassing, sealing was performed, and HIP treatment was performed under the conditions of 1250 ° C. × 2 hours and 1000 atm. The density of the sintered body obtained at this time is 80 to 85 in relative density.
%.
この後、HIP缶ごと焼結体を1300℃の温度で１回の加
工率10〜30％で断面が1100×330mmで厚みが10mmの寸法
になるまで熱間圧延を数回繰り返した。圧延後、1200℃
で歪取り焼鈍により加工歪を除去した。得られた圧延材
をHIP缶除去後、所定の形状に機械加工し、φ300mmのタ
ーゲットを得た。Thereafter, the sintered body together with the HIP can was subjected to hot rolling several times at a temperature of 1300 [deg.] C., a processing rate of 10 to 30%, a cross section of 1100 * 330 mm and a thickness of 10 mm. After rolling, 1200 ° C
The work strain was removed by strain relief annealing. After the obtained rolled material was removed from the HIP can, it was machined into a predetermined shape to obtain a φ300 mm target.
得られたターゲットの平均粒径は７μｍであった。ま
た相対密度は99.9％以上でほぼ理論密度と同一の値であ
った。純度的には製造工程中の汚染はなく、Ｗ≧99.999
％〔放射性元素含有量3ppb以下、アルカリ金属含有量10
0ppb以下であった。〕、酸素は230ppmと低い値であっ
た。The average particle size of the obtained target was 7 μm. The relative density was 99.9% or more, almost the same value as the theoretical density. In terms of purity, there is no contamination during the manufacturing process and W ≧ 99.999
% [Radioactive element content 3 ppb or less, alkali metal content 10
It was less than 0 ppb. ] And oxygen was as low as 230 ppm.
本ターゲットで形成したスパッタリング膜は均一であ
り、かつパーティクル数が50ケ/6inchウェハーであっ
た。The sputtering film formed with this target was uniform, and the number of particles was 50/6 inch wafer.
（比較例） 高純度タングステン粉末（Ｗ≧99.999％〔放射性元素
含有量3ppb以下、アルカリ金属含有量100ppb以下〕、粒
度FSSS（フィッシャー粒度）で５μｍ以下）を内径φ40
0mmのダイスに充填し、1400℃×300kg/cm2×0.5時間の
条件でホットプレスした。得られたホットプレス体を切
削加工し、φ300mmのターゲットを得た。ターゲットの
相対密度は83％であった。(Comparative Example) High-purity tungsten powder (W ≧ 99.999% [radioactive element content 3 ppb or less, alkali metal content 100 ppb or less], particle size FSSS (Fisher particle size) 5 μm or less) with an inner diameter of φ40
A 0 mm die was filled and hot-pressed at 1400 ° C. × 300 kg / cm 2 × 0.5 hours. The obtained hot pressed body was cut to obtain a target of φ300 mm. The relative density of the target was 83%.
本ターゲットで形成したスパッタリング膜中のパーテ
ィクル数は、200ヶ以上/6inchウェハーで著しく多く、
ウェハー歩留低下の原因となった。The number of particles in the sputtering film formed with this target is remarkably large for 200 or more / 6-inch wafers.
This caused a decrease in wafer yield.
以上説明のように、本発明によると微細組織であり、
かつ相対密度99％以上の高純度のタングステンターゲッ
トを得ることができる。したがって、ターゲットを機械
加工する場合に割れを生じることもなく、スパッタリン
グにおいても焼結粒の異方性がないため、均一な膜を形
成し、かつ膜中のパーティクル数を著しく低減し、ウェ
ハー歩留りが向上する。As described above, according to the present invention is a microstructure,
In addition, a high-purity tungsten target having a relative density of 99% or more can be obtained. Therefore, when the target is machined, there is no crack, and since there is no anisotropy of the sintered grains even in sputtering, a uniform film is formed, and the number of particles in the film is significantly reduced. Is improved.
Claims (1)
予備焼結体を製造し、ついで1200℃以上で熱間塑性加工
して相対密度99％以上を得ることを特徴とするタングス
テンターゲットの製造方法。1. Production of a tungsten target characterized in that a pre-sintered body is produced using a high-purity tungsten powder raw material, and then hot plastic working is performed at 1200 ° C. or more to obtain a relative density of 99% or more. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1286699A JP2757287B2 (en) | 1989-11-02 | 1989-11-02 | Manufacturing method of tungsten target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1286699A JP2757287B2 (en) | 1989-11-02 | 1989-11-02 | Manufacturing method of tungsten target |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP00715398A Division JP3244167B2 (en) | 1998-01-19 | 1998-01-19 | Tungsten or molybdenum target |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03150356A JPH03150356A (en) | 1991-06-26 |
| JP2757287B2 true JP2757287B2 (en) | 1998-05-25 |
Family
ID=17707842
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1286699A Expired - Lifetime JP2757287B2 (en) | 1989-11-02 | 1989-11-02 | Manufacturing method of tungsten target |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2757287B2 (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995016797A1 (en) * | 1993-12-14 | 1995-06-22 | Kabushiki Kaisha Toshiba | Molybdenum-tungsten material for wiring, molybdenum-tungsten target for wiring, process for producing the same, and molybdenum-tungsten wiring thin film |
| JP4634567B2 (en) * | 2000-04-17 | 2011-02-16 | 株式会社東芝 | Method for manufacturing tungsten sputtering target |
| JP4900992B2 (en) * | 2000-07-21 | 2012-03-21 | 株式会社東芝 | Sputtering target and Ge layer, Ge compound layer, Ge alloy layer and optical disk, electric / electronic component, magnetic component using the sputtering target |
| US20070243095A1 (en) * | 2004-06-15 | 2007-10-18 | Tosoh Smd, Inc. | High Purity Target Manufacturing Methods |
| US20060042728A1 (en) * | 2004-08-31 | 2006-03-02 | Brad Lemon | Molybdenum sputtering targets |
| US8088232B2 (en) | 2004-08-31 | 2012-01-03 | H.C. Starck Inc. | Molybdenum tubular sputtering targets with uniform grain size and texture |
| JP5443403B2 (en) * | 2004-09-30 | 2014-03-19 | 株式会社神戸製鋼所 | Hard coating excellent in high temperature lubricity and wear resistance and target for forming the hard coating |
| AT8697U1 (en) | 2005-10-14 | 2006-11-15 | Plansee Se | TUBE TARGET |
| DE102005050424B4 (en) * | 2005-10-19 | 2009-10-22 | W.C. Heraeus Gmbh | Sputtering target made of multi-component alloys |
| US20110094879A1 (en) | 2008-06-02 | 2011-04-28 | Jx Nippon Mining & Metals Corporation | Tungsten Sintered Sputtering Target |
| JP4797099B2 (en) | 2009-10-01 | 2011-10-19 | Ｊｘ日鉱日石金属株式会社 | Manufacturing method of high purity tungsten powder |
| JP5550328B2 (en) * | 2009-12-22 | 2014-07-16 | 株式会社東芝 | Mo sputtering target and manufacturing method thereof |
| CN102699626A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Fabricating technique of tungsten plane targets |
| WO2014069328A1 (en) * | 2012-11-02 | 2014-05-08 | Jx日鉱日石金属株式会社 | Tungsten sintered body sputtering target and tungsten film formed using said target |
| JP7308013B2 (en) * | 2017-11-10 | 2023-07-13 | Ｊｘ金属株式会社 | Tungsten sputtering target and manufacturing method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62174373A (en) * | 1985-10-04 | 1987-07-31 | Hitachi Metals Ltd | Chromium target material and its production |
| JPS63216966A (en) * | 1987-03-06 | 1988-09-09 | Toshiba Corp | spatuta target |
-
1989
- 1989-11-02 JP JP1286699A patent/JP2757287B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03150356A (en) | 1991-06-26 |
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