WO2016129449A1 - Cr-Ti合金スパッタリングターゲット材およびその製造方法 - Google Patents
Cr-Ti合金スパッタリングターゲット材およびその製造方法 Download PDFInfo
- Publication number
- WO2016129449A1 WO2016129449A1 PCT/JP2016/053020 JP2016053020W WO2016129449A1 WO 2016129449 A1 WO2016129449 A1 WO 2016129449A1 JP 2016053020 W JP2016053020 W JP 2016053020W WO 2016129449 A1 WO2016129449 A1 WO 2016129449A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- mass ppm
- target material
- sputtering target
- alloy sputtering
- powder
- Prior art date
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/62—Record carriers characterised by the selection of the material
- G11B5/73—Base layers, i.e. all non-magnetic layers lying under a lowermost magnetic recording layer, e.g. including any non-magnetic layer in between a first magnetic recording layer and either an underlying substrate or a soft magnetic underlayer
- G11B5/7368—Non-polymeric layer under the lowermost magnetic recording layer
- G11B5/7373—Non-magnetic single underlayer comprising chromium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/06—Alloys based on chromium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/851—Coating a support with a magnetic layer by sputtering
Definitions
- the present invention relates to a Cr—Ti alloy sputtering target material for forming a Cr—Ti alloy layer used as an underlayer of a magnetic recording medium, and a method for producing the same.
- Hard disk drives have been actively studied to increase the density of magnetic recording media due to their smaller size and larger capacity.
- perpendicular magnetic recording has been put to practical use as a method that can achieve higher recording densities. And has become mainstream.
- new recording methods such as patterned media and heat-assisted recording are being developed.
- the perpendicular magnetic recording system is a magnetic film of a perpendicular magnetic recording medium formed so that the easy axis of magnetization is oriented perpendicular to the medium surface, and even if the recording density is increased, the demagnetizing field in the bit is small, This method is suitable for increasing the recording density with little deterioration in recording / reproducing characteristics.
- a perpendicular magnetic recording medium generally has a multilayer structure having a base layer / soft magnetic backing layer / seed layer / Ru intermediate layer / CoPtCr—SiO 2 magnetic layer / protective layer on a substrate made of glass or aluminum.
- a Cr—Ti layer is formed on a part of the base layer.
- the multilayer structure of the perpendicular magnetic recording medium is formed by film formation using a magnetron sputtering method. With magnetron sputtering, permanent magnets are placed on the back of a base material called a sputtering target material. It is a method to do.
- the magnetic recording medium is manufactured using a sputtering apparatus provided with an independent film forming chamber for each layer.
- the sputtering target material is a plate material adjusted to a desired thin film composition, and is generally manufactured by a melt casting method or a powder sintering method.
- the Cr—Ti alloy sputtering target material used for forming the Cr—Ti layer is manufactured by a powder sintering method.
- the Cr—Ti alloy sputtering target material easily forms an intermetallic compound phase (TiCr 2 phase) having a lower sputtering rate than that of a pure Cr phase or a pure Ti phase during sintering.
- the TiCr 2 phase generates massive foreign substances called particles, and the particles adhere to the recording medium on which the film is formed, thereby reducing the product yield.
- the Cr—Ti alloy sputtering target material disclosed in Patent Document 1 described above is effective in reducing the generation of coarse particles due to the TiCr 2 phase.
- fine particles that have not previously affected the quality of recording media have contributed to a reduction in product yield.
- An object of the present invention is to provide a Cr—Ti alloy sputtering target material and a method for producing the same that can solve the above-described problems and can suppress the generation of fine particles during sputtering.
- the present inventor has found that the composition formula in atomic ratio is represented by Cr 100-X 2 -Ti X , 40 ⁇ X ⁇ 60, and the balance is Cr—Ti alloy sputtering target material composed of inevitable impurities.
- the impurities contained, Mg, Al, Si, Mn, Ni, Cu and Sn were the starting points for nodule generation.
- a high-purity Cr—Ti alloy sputtering target material in which these impurities are controlled within a specific range it is possible to suppress the generation of nodules, and Ti with reduced element content.
- a Cr—Ti alloy sputtering target material can be produced using powder and Cr powder, and the present invention has been achieved.
- the present invention can suppress the generation of fine particles during sputtering by suppressing the generation of the nodules.
- the composition formula in atomic ratio is represented by Cr 100-X -Ti X , 40 ⁇ X ⁇ 60, and the balance is unavoidable impurities, and among these impurities, Mg, Al, Si, Mn, It is a Cr—Ti alloy sputtering target material containing Ni, Cu and Sn in a total of 1 mass ppm to 50 mass ppm.
- the Cr—Ti alloy sputtering target material of the present invention has Mg ⁇ 1 mass ppm, Al ⁇ 10 mass ppm, Si ⁇ 10 mass ppm, Mn ⁇ 1 mass ppm, Ni ⁇ 10 mass ppm, Cu ⁇ 1 mass ppm, It is preferable that Sn ⁇ 5 mass ppm.
- the Cr—Ti alloy sputtering target material of the present invention includes, as impurities, Ti powder containing Mg, Al, Si, Mn, Ni, Cu, and Sn in a total amount of 1 mass ppm to 50 mass ppm, and impurities.
- Mg, Al, Si, Mn, Ni, Cu, and Sn are mixed with Cr powder containing 1 mass ppm or more and 50 mass ppm or less in total, and can be obtained by pressure sintering.
- the Ti powder has Mg ⁇ 1 mass ppm, Al ⁇ 2 mass ppm, Si ⁇ 10 mass ppm, Mn ⁇ 2 mass ppm, Ni ⁇ 10 mass ppm, Cu ⁇ 10 mass ppm, and Sn ⁇ 2 mass ppm. preferable.
- the Cr powder has Mg ⁇ 1 mass ppm, Al ⁇ 10 mass ppm, Si ⁇ 10 mass ppm, Mn ⁇ 1 mass ppm, Ni ⁇ 10 mass ppm, Cu ⁇ 1 mass ppm, and Sn ⁇ 10 mass ppm. It is preferable.
- the present invention can provide a Cr—Ti alloy sputtering target material capable of suppressing the generation of fine particles during sputtering and a method for manufacturing the same, and is a useful technique for manufacturing a magnetic recording medium.
- FIG. 2 is a secondary electron image of a scanning electron microscope of the Cr—Ti alloy sputtering target material of Example 1 of the present invention.
- 6 is a secondary electron image of a scanning electron microscope of the Cr—Ti alloy sputtering target material of Example 2 of the present invention.
- 2 is a secondary electron image of a scanning electron microscope of the Cr—Ti alloy sputtering target material of Comparative Example 1.
- FIG. 4 is a secondary electron image of a scanning electron microscope of a Cr—Ti alloy sputtering target material of Comparative Example 2.
- compositional formula in terms of atomic ratio is expressed by Cr 100-X -Ti X , 40 ⁇ X ⁇ 60, and the balance in order to suppress generation of nodules that are the starting points of particles during sputtering.
- Mg, Al, Si, Mn, Ni, Cu, and Sn are controlled to a specific range as impurities of the Cr—Ti alloy sputtering target material composed of inevitable impurities.
- the present invention is characterized in that, in order to produce this Cr—Ti alloy sputtering target material, Ti powder and Cr powder, in which each of the above impurities is controlled within a specific range, are mixed and pressure-sintered. Have.
- the composition formula in atomic ratio is represented by Cr 100-X —Ti X , 40 ⁇ X ⁇ 60, and the balance is made of inevitable impurities.
- the Ti content is such that when a Cr—Ti alloy is used as a part of the underlayer or seed layer of the magnetic recording medium, it is possible to form a thin film with high thin film adhesion and good crystallinity, This is defined as a range in which a magnetic recording medium having high recording / reproducing characteristics can be manufactured.
- the Cr—Ti alloy sputtering target material of the present invention has a total content of these impurities of 1 from the viewpoint of controlling Mg, Al, Si, Mn, Ni, Cu, and Sn as impurities as starting points of nodules to a very small amount. It is defined as not less than mass ppm and not more than 50 mass ppm.
- the total content of impurities is preferably 1 to 17 ppm by mass, and more preferably 1 to 13 ppm by mass.
- Ni forms a Ni—Ti compound with a low sputtering rate especially during the refining process of Ti, and therefore tends to be the starting point of abnormal discharge during sputtering, which causes nodule generation. For this reason, in the Cr—Ti alloy sputtering target material of the present invention, Ni ⁇ 10 mass ppm is preferable.
- Mg, Al, Si and Mn have a high affinity with oxygen. If they are contained in a large amount in the Ti powder or Cr powder of the raw material powder, the raw material powder is stored and manufactured. In the process, an oxide is easily formed. These oxides are chemically bonded stably, have a lower sputtering rate than the surrounding metal structure, and tend to be the starting point of nodules. For this reason, in the Cr—Ti alloy sputtering target material of the present invention, Mg ⁇ 1 mass ppm, Al ⁇ 10 mass ppm, Si ⁇ 10 mass ppm, and Mn ⁇ 1 mass ppm are preferable.
- impurities Cu and Sn each form a liquid phase at 500 ° C. or less, which is the surface temperature of the sputtering target material in sputtering, and are likely to be the starting point of nodules.
- Cu ⁇ 1 mass ppm and Sn ⁇ 5 mass ppm are preferable.
- the Cr—Ti alloy sputtering target material of the present invention inevitably contains these impurities even from the viewpoint of controlling Mg, Al, Si, Mn, Ni, Cu, and Sn to a very small amount.
- the lower limit is 1 mass ppm or more in total.
- the inevitable metal impurities excluding gas components other than Mg, Al, Si, Mn, Ni, Cu and Sn are preferably 100 ppm by mass or less in total. .
- the above-described Cr—Ti alloy sputtering target material of the present invention comprises Ti powder and Cr powder containing Mg, Al, Si, Mn, Ni, Cu and Sn as impurities in a total of 1 mass ppm to 50 mass ppm. It can be obtained by mixing and pressure sintering. Since the Ti powder used as the raw material powder is manufactured through sponge Ti that is generally manufactured by a crawl method, it easily contains impurities such as Mg, Al, and Si. For this reason, the Ti powder used in the present invention is a Ti raw material ingot obtained by pressure-molding the above sponge Ti into a briquette shape as a raw material, and further refining the molded body by vacuum arc melting or the like. Is preferably used.
- the obtained Ti powder is Mg ⁇ 1 mass ppm, Al ⁇ 2 mass ppm, Si ⁇ 10 mass ppm, Mn ⁇ 2 mass ppm, Ni ⁇ 10 mass ppm, Cu ⁇ 10 mass ppm, Sn ⁇ 2 mass ppm. Controlled.
- the Ti powder used in the present invention Fe contained as impurities is controlled to 100 mass ppm or less and oxygen is controlled to 900 mass ppm or less in order to suppress generation of coarse particles which has been a problem in the past. It is more preferable.
- the Ti powder preferably has a particle size of 100 mesh or less and 325 mesh or more. Thereby, the Cr—Ti alloy sputtering target material of the present invention can reduce the TiCr 2 phase that contributes to coarse particles.
- the Cr powder used as the raw material powder in the present invention is a reduction heat treatment of a high-purity electrolytic Cr pulverized powder in a hydrogen atmosphere.
- the obtained Cr powder is Mg ⁇ 1 mass ppm, Al ⁇ 10 mass ppm, Si ⁇ 10 mass ppm, Mn ⁇ 1 mass ppm, Ni ⁇ 10 mass ppm, Cu ⁇ 1 mass ppm, Sn ⁇ 10 mass ppm. Controlled.
- the Cr powder used in the present invention preferably has a particle size of 32 mesh or less and 325 mesh or more. Thereby, in the Cr—Ti alloy sputtering target material of the present invention, the TiCr 2 phase is reduced, and generation of coarse particles can be suppressed.
- a hot isostatic pressing method, a hot pressing method, an electric current sintering method, or the like can be applied.
- a sintered body in which the formation of the TiCr 2 phase is sufficiently suppressed can be obtained.
- the pressure by setting the pressure to 20 MPa or more, good sintering can be achieved without impairing the sintered density.
- the Ti powder used in Example 1 of the present invention is a Ti powder produced by collecting debris from a Ti raw material ingot obtained by vacuum refining sponge Ti, hydrogenating and crushing it once, and then subjecting it to dehydrogenation treatment. Prepared by sieving and classifying with a mesh sieve. Further, the Ti powder used in Invention Example 2 is obtained by dissolving the Ti raw material ingot and sieving and classifying the Ti powder produced by a non-contact type inert gas atomizing method using no refractory with a 100 mesh sieve. And prepared.
- Each powder prepared above was mixed so that the atomic ratio was Cr 55 -Ti 45 , filled into a soft iron capsule, degassed and sealed, and then at a temperature of 850 ° C., a holding pressure of 120 MPa, and a holding time of 1 hour.
- the sintered body was manufactured by pressure sintering with a hot isostatic press under conditions.
- the obtained sintered body was machined to a diameter of 180 mm and a thickness of 10 mm to prepare a Cr—Ti alloy sputtering target material.
- Comparative Example 1 a commercially available Ti powder having a purity of 99.9% by mass and the above Cr powder were mixed so as to have an atomic ratio of Cr 55 —Ti 45, and pressure sintered under the same sintering conditions as above.
- a Cr—Ti alloy sputtering target material was prepared.
- Comparative Example 2 after the sponge Ti was once hydrogenated and pulverized, the Ti powder produced by performing the dehydrogenation treatment and the above Cr powder were mixed so that the atomic ratio was Cr 50 -Ti 50 , A Cr—Ti alloy sputtering target material pressure-sintered under the same sintering conditions as described above was prepared.
- Each of the Cr—Ti alloy sputtering target materials prepared above was placed in the chamber of a DC magnetron sputtering apparatus (model: C3010) manufactured by Canon Anelva Inc., and the pressure in the chamber was reduced to 1 ⁇ 10 ⁇ 6 Pa or less. Thereafter, sputtering was performed for 5 hours under the conditions of Ar gas pressure of 0.3 Pa and input power of 1500 W. Next, the 157 ⁇ m ⁇ 209 ⁇ m field of view of the sputtering surface of each Cr—Ti alloy sputtering target material was observed with a scanning electron microscope (model: S-3600N) manufactured by Hitachi High-Technologies Corporation at a magnification of 600 times. The number of nodules whose major axis was confirmed to be 5.0 ⁇ m or more and the number of nodules whose major axis was 0.1 ⁇ m or more and less than 5.0 ⁇ m were measured. The measurement results are shown in Table 2.
- FIGS. 3 and 4 show Comparative Example 1 and Comparative Example 2.
- the secondary electron image of the sputtering surface after the sputtering of the Cr—Ti alloy sputtering target material is shown.
- 9 and 8 nodules each having a major axis of 5.0 ⁇ m or more were detected on the sputtering surface, and the numbers of nodules having a major axis of 0.1 ⁇ m or more and less than 5.0 ⁇ m were 24 or 47, respectively. Remarkably many were confirmed.
- Invention Example 1 and Invention Example 2 each have 0 nodules with a major axis of 5.0 ⁇ m or more and 0 nodules with a major axis of 0.1 ⁇ m or more and less than 5.0 ⁇ m, respectively.
- the effectiveness of the present invention was confirmed.
- generation of fine particles can be suppressed during sputtering using the material.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
- Powder Metallurgy (AREA)
- Magnetic Record Carriers (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
Description
しかし、Cr-Ti合金スパッタリングターゲット材は、焼結時に純Cr相や純Ti相に比べてスパッタ率の低い金属間化合物相(TiCr2相)を形成しやすい。このTiCr2相は、パーティクルと呼ばれる塊状異物を発生させてしまい、そのパーティクルが成膜された記録媒体上に付着することで製品歩留を低下させてしまう。このため、Cr-Ti合金スパッタリングターゲット材の組織の改良が試みられている。例えば、Tiを40~60原子%含有するCr-Ti合金スパッタリングターゲット材において、粉末焼結時に形成されるTiCr2相を微量に制御することで、スパッタリング時に発生するパーティクルを低減できることが提案されている。
しかしながら、昨今の磁気記録媒体の高記録密度化に伴って、従来は記録媒体の品位に影響しなかった微細なパーティクルが製品歩留を低下させる一因となっている。
本発明者は、特許文献1に記載されたCr-Ti合金スパッタリングターゲット材をスパッタリングしたところ、スパッタリングターゲット材から微細なパーティクルが多数発生することを確認した。そして、その主原因として、スパッタリングターゲット材のスパッタ面にノジュールと呼ばれる長径が0.1μm以上5.0μm未満の微小な突起物が局部的に発生する現象を確認した。
本発明の目的は、上記課題を解決し、スパッタリング時に、微細なパーティクルが発生することを抑制可能なCr-Ti合金スパッタリングターゲット材およびその製造方法を提供することである。
また、本発明のCr-Ti合金スパッタリングターゲット材は、Mg≦1質量ppm、Al≦10質量ppm、Si≦10質量ppm、Mn≦1質量ppm、Ni≦10質量ppm、Cu≦1質量ppm、Sn≦5質量ppmであることが好ましい。
前記Ti粉末は、Mg≦1質量ppm、Al≦2質量ppm、Si≦10質量ppm、Mn≦2質量ppm、Ni≦10質量ppm、Cu≦10質量ppm、Sn≦2質量ppmであることが好ましい。
また、前記Cr粉末は、Mg≦1質量ppm、Al≦10質量ppm、Si≦10質量ppm、Mn≦1質量ppm、Ni≦10質量ppm、Cu≦1質量ppm、Sn≦10質量ppmであることが好ましい。
そして、本発明は、このCr-Ti合金スパッタリングターゲット材を製造するために、上記の各不純物を特定の範囲に制御したTi粉末とCr粉末とを混合し、加圧焼結することに特徴を有している。
上記Tiの含有量は、磁気記録媒体の下地層やシード層の一部としてCr-Ti合金を使用した際に、薄膜の密着性が高く、結晶性のよい薄膜を形成することが可能で、高い記録再生特性を有する磁気記録媒体を製造することが可能な範囲として規定するものである。
上述の不純物の中で、Niは、特にTiの精錬過程において、スパッタ率が小さいNi-Ti化合物を形成してしまうため、スパッタリング時に異常放電の起点となりやすく、ノジュール発生の原因となる。このため、本発明のCr-Ti合金スパッタリングターゲット材では、Ni≦10質量ppmにすることが好ましい。
尚、本発明のCr-Ti合金スパッタリングターゲット材は、Mg、Al、Si、Mn、Ni、CuおよびSnを極微量に制御する観点であっても、これら不純物は不可避的に含まれるものがあり、その下限は合計で1質量ppm以上である。
また、本発明のCr-Ti合金スパッタリングターゲット材は、Mg、Al、Si、Mn、Ni、CuおよびSn以外のガス成分を除く不可避の金属不純物は、合計で100質量ppm以下にすることが好ましい。
原料粉末として用いるTi粉末は、一般的にクロール法によって製造されるスポンジTiを経て製造されるために、Mg、Al、Siなどの不純物を含有しやすい。このため、本発明で用いるTi粉末は、原料として、上記のスポンジTiをブリケット状に加圧成型して成型体とし、さらに、この成型体を真空アーク溶解等により2次精錬したTi原料鋳塊を用いることが好ましい。そして、この2次精錬したTi原料鋳塊から切削屑を採取し、一旦水素化して粉砕した後に脱水素処理を施してTi粉末を得ることが好ましい。これにより、得られるTi粉末は、Mg≦1質量ppm、Al≦2質量ppm、Si≦10質量ppm、Mn≦2質量ppm、Ni≦10質量ppm、Cu≦10質量ppm、Sn≦2質量ppmに制御される。
尚、耐火物を用いない非接触型の不活性ガスアトマイズ法に、上記の2次精錬したTi原料鋳塊を適用して製造することでも、Ti粉末の不純物量を上記の範囲に制御することが可能である。
また、本発明で用いるTi粉末は、従来より問題となっていた粗大なパーティクルの発生を抑制するために、不純物として含まれるFeを100質量ppm以下、酸素を900質量ppm以下に制御されていることがより好ましい。また、Ti粉末は、100メッシュ以下、且つ325メッシュ以上の粒径であることが好ましい。これにより、本発明のCr-Ti合金スパッタリングターゲット材は、粗大なパーティクルの一因となるTiCr2相を低減することができる。
また、32メッシュ以下のCr粉末を使用することにより、本発明のスパッタリングターゲット材の組織中に粗大な純Cr相の残存を抑制することができる。また、325メッシュ以上の粒径のCr粉末を用いることにより、比表面積の増大を抑制して、粗大なパーティクルの一因となる、Tiとの粒界に形成されるTiCr2相を抑制することができる。このため、本発明で用いるCr粉末は、32メッシュ以下、且つ325メッシュ以上の粒径にすることが好ましい。これにより、本発明のCr-Ti合金スパッタリングターゲット材は、TiCr2相が低減され、粗大なパーティクルの発生を抑制することができる。
上記で準備した各粉末を、原子比でCr55-Ti45となるように混合し、軟鉄製のカプセルに充填し、脱ガス封止した後に温度850℃、保持圧力120MPa、保持時間1時間の条件で熱間静水圧プレスによって加圧焼結し、焼結体を製造した。
得られた焼結体を直径180mm、厚さ10mmに機械加工してCr-Ti合金スパッタリングターゲット材を作製した。
次いで、各Cr-Ti合金スパッタリングターゲット材のスパッタ面について、株式会社日立ハイテクノロジーズ社製の走査型電子顕微鏡(型式:S-3600N)を用いて、600倍の倍率で観察した157μm×209μmの視野において確認された長径が5.0μm以上のノジュール数、および長径が0.1μm以上5.0μm未満のノジュールの数を測定した。測定結果を表2に示す。
比較例1および比較例2は、スパッタ面に長径5.0μm以上のノジュールがそれぞれ9個と8個検出されており、長径0.1μm以上5.0μm未満のノジュール数がそれぞれ24個、47個と顕著に多く確認された。
一方、本発明例1および本発明例2は、長径5.0μm以上のノジュールがそれぞれ0個、長径0.1μm以上5.0μm未満のノジュール数もそれぞれ0個であり、ノジュールの発生が大幅に低減されており、本発明の有効性が確認できた。本発明のCr-Ti合金スパッタリングターゲット材によれば、これを用いたスパッタリング時に、微細なパーティクルの発生を抑制することができる。
Claims (5)
- 原子比における組成式がCr100-X-TiX、40≦X≦60で表わされ、残部が不可避的不純物からなり、前記不純物のうちMg、Al、Si、Mn、Ni、CuおよびSnを合計で1質量ppm以上50質量ppm以下含有することを特徴とするCr-Ti合金スパッタリングターゲット材。
- 請求項1において、Mg≦1質量ppm、Al≦10質量ppm、Si≦10質量ppm、Mn≦1質量ppm、Ni≦10質量ppm、Cu≦1質量ppm、Sn≦5質量ppmであることを特徴とするCr-Ti合金スパッタリングターゲット材。
- 不純物として、Mg、Al、Si、Mn、Ni、Cu、およびSnを合計で1質量ppm以上50質量ppm以下含有するTi粉末と、不純物として、Mg、Al、Si、Mn、Ni、Cu、およびSnを合計で1質量ppm以上50質量ppm以下含有するCr粉末とを混合し、加圧焼結することにより、原子比における組成式がCr100-X-TiX、40≦X≦60で表わされ、残部が不可避的不純物からなり、前記不純物のうちMg、Al、Si、Mn、Ni、CuおよびSnを合計で1質量ppm以上50質量ppm以下含有するCr-Ti合金スパッタリングターゲット材を得ることを特徴とするCr-Ti合金スパッタリングターゲット材の製造方法。
- 請求項3において、前記Ti粉末は、Mg≦1質量ppm、Al≦2質量ppm、Si≦10質量ppm、Mn≦2質量ppm、Ni≦10質量ppm、Cu≦10質量ppm、Sn≦2質量ppmであることを特徴とするCr-Ti合金スパッタリングターゲット材の製造方法。
- 請求項4において、前記Cr粉末は、Mg≦1質量ppm、Al≦10質量ppm、Si≦10質量ppm、Mn≦1質量ppm、Ni≦10質量ppm、Cu≦1質量ppm、Sn≦10質量ppmであることを特徴とするCr-Ti合金スパッタリングターゲット材の製造方法。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2016574745A JP6312009B2 (ja) | 2015-02-12 | 2016-02-02 | Cr−Ti合金スパッタリングターゲット材およびその製造方法 |
CN201680009216.1A CN107208259B (zh) | 2015-02-12 | 2016-02-02 | 铬-钛合金溅射靶材及其制造方法 |
MYPI2017702896A MY180072A (en) | 2015-02-12 | 2016-02-02 | Cr-ti alloy sputtering target material and method for producing same |
SG11201706280XA SG11201706280XA (en) | 2015-02-12 | 2016-02-02 | Cr-Ti ALLOY SPUTTERING TARGET MATERIAL AND METHOD FOR PRODUCING SAME |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015025303 | 2015-02-12 | ||
JP2015-025303 | 2015-02-12 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2016129449A1 true WO2016129449A1 (ja) | 2016-08-18 |
Family
ID=56614648
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2016/053020 WO2016129449A1 (ja) | 2015-02-12 | 2016-02-02 | Cr-Ti合金スパッタリングターゲット材およびその製造方法 |
Country Status (6)
Country | Link |
---|---|
JP (1) | JP6312009B2 (ja) |
CN (1) | CN107208259B (ja) |
MY (1) | MY180072A (ja) |
SG (1) | SG11201706280XA (ja) |
TW (1) | TW201631170A (ja) |
WO (1) | WO2016129449A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPWO2018131328A1 (ja) * | 2017-01-12 | 2019-11-07 | 日立金属株式会社 | Cr合金ターゲット材 |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111438355B (zh) * | 2020-04-13 | 2022-02-22 | 河北晟华新材料科技有限公司 | 一种铬铝硅靶材及其制备方法 |
CN112517917B (zh) * | 2020-11-25 | 2023-04-18 | 河南东微电子材料有限公司 | 一种用于铬钛靶材的CrTiLa合金粉末的制备方法 |
CN112813326A (zh) * | 2020-12-29 | 2021-05-18 | 有研工程技术研究院有限公司 | 一种钛铝铬合金靶及其制备方法 |
TWI769081B (zh) * | 2021-09-17 | 2022-06-21 | 光洋應用材料科技股份有限公司 | 鉻鎳鈦合金靶材及其製法 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011252227A (ja) * | 2010-05-06 | 2011-12-15 | Hitachi Metals Ltd | Cr−Ti合金ターゲット材 |
JP2012041585A (ja) * | 2010-08-17 | 2012-03-01 | Sanyo Special Steel Co Ltd | CrTi系合金およびスパッタリング用ターゲット材並びにそれらを使用した垂直磁気記録媒体の製造方法 |
WO2013038962A1 (ja) * | 2011-09-14 | 2013-03-21 | Jx日鉱日石金属株式会社 | 高純度銅マンガン合金スパッタリングターゲット |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3002265B2 (ja) * | 1990-12-12 | 2000-01-24 | 日本重化学工業株式会社 | 高純度金属クロムの製造方法 |
US5866067A (en) * | 1997-03-24 | 1999-02-02 | Sony Corporation And Materials Research Corporation | High purity chromium metal by casting with controlled oxygen content |
US6063254A (en) * | 1997-04-30 | 2000-05-16 | The Alta Group, Inc. | Method for producing titanium crystal and titanium |
US6309595B1 (en) * | 1997-04-30 | 2001-10-30 | The Altalgroup, Inc | Titanium crystal and titanium |
-
2016
- 2016-02-02 MY MYPI2017702896A patent/MY180072A/en unknown
- 2016-02-02 SG SG11201706280XA patent/SG11201706280XA/en unknown
- 2016-02-02 CN CN201680009216.1A patent/CN107208259B/zh active Active
- 2016-02-02 WO PCT/JP2016/053020 patent/WO2016129449A1/ja active Application Filing
- 2016-02-02 JP JP2016574745A patent/JP6312009B2/ja active Active
- 2016-02-03 TW TW105103474A patent/TW201631170A/zh unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011252227A (ja) * | 2010-05-06 | 2011-12-15 | Hitachi Metals Ltd | Cr−Ti合金ターゲット材 |
JP2012041585A (ja) * | 2010-08-17 | 2012-03-01 | Sanyo Special Steel Co Ltd | CrTi系合金およびスパッタリング用ターゲット材並びにそれらを使用した垂直磁気記録媒体の製造方法 |
WO2013038962A1 (ja) * | 2011-09-14 | 2013-03-21 | Jx日鉱日石金属株式会社 | 高純度銅マンガン合金スパッタリングターゲット |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPWO2018131328A1 (ja) * | 2017-01-12 | 2019-11-07 | 日立金属株式会社 | Cr合金ターゲット材 |
JP7103233B2 (ja) | 2017-01-12 | 2022-07-20 | 日立金属株式会社 | Cr合金ターゲット材 |
Also Published As
Publication number | Publication date |
---|---|
JPWO2016129449A1 (ja) | 2017-11-24 |
SG11201706280XA (en) | 2017-09-28 |
TWI561638B (ja) | 2016-12-11 |
MY180072A (en) | 2020-11-20 |
CN107208259A (zh) | 2017-09-26 |
CN107208259B (zh) | 2019-08-13 |
TW201631170A (zh) | 2016-09-01 |
JP6312009B2 (ja) | 2018-04-18 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP6312009B2 (ja) | Cr−Ti合金スパッタリングターゲット材およびその製造方法 | |
JP2005320627A (ja) | Co合金ターゲット材の製造方法、Co合金ターゲット材および垂直磁気記録用軟磁性膜ならびに垂直磁気記録媒体 | |
JPWO2013108520A1 (ja) | Co−Cr−Pt系スパッタリングターゲット及びその製造方法 | |
JP5370917B2 (ja) | Fe−Co−Ni系合金スパッタリングターゲット材の製造方法 | |
JP6262332B2 (ja) | Al−Te−Cu−Zr合金からなるスパッタリングターゲット及びその製造方法 | |
JP2020147851A (ja) | 磁気記録媒体用スパッタリングターゲット及び磁性薄膜 | |
JP6005767B2 (ja) | 磁性記録媒体用スパッタリングターゲット | |
JP2009191359A (ja) | Fe−Co−Zr系合金ターゲット材 | |
JP5854308B2 (ja) | Cr−Ti合金ターゲット材 | |
JPWO2016133047A1 (ja) | 磁性体薄膜形成用スパッタリングターゲット | |
JP3525439B2 (ja) | ターゲット部材およびその製造方法 | |
WO2021141042A1 (ja) | スパッタリングターゲット材の製造方法 | |
JP7153729B2 (ja) | スパッタリングターゲット及び磁性膜 | |
JP7157573B2 (ja) | 磁気記録媒体のシード層用Ni系合金 | |
JP5646757B2 (ja) | 強磁性材スパッタリングターゲット | |
JP6575775B2 (ja) | 軟磁性膜 | |
JP7317741B2 (ja) | スパッタリングターゲット、磁性膜、及びスパッタリングターゲット作製用の原料混合粉末 | |
WO2017141558A1 (ja) | 磁気記録媒体用スパッタリングターゲット及び磁性薄膜 | |
JP7274361B2 (ja) | 磁気記録媒体のシード層用合金 | |
JP2013028841A (ja) | 酸化コバルト及び非磁性酸化物を有するCoCrPtに基づく合金スパッタリングターゲット及びその製造法 | |
JP2021109979A (ja) | スパッタリングターゲット材 | |
JP2021180057A (ja) | スパッタリングターゲット材 | |
JP2022177530A (ja) | 磁気記録媒体の密着膜層用CrTi系合金、スパッタリングターゲット材及び垂直磁気記録媒体 | |
JP2018172762A (ja) | スパッタリングターゲット、磁性膜および、磁性膜の製造方法 | |
JPH05247641A (ja) | ターゲット部材およびその製造方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 16749093 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 2016574745 Country of ref document: JP Kind code of ref document: A |
|
WWE | Wipo information: entry into national phase |
Ref document number: 11201706280X Country of ref document: SG |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
122 | Ep: pct application non-entry in european phase |
Ref document number: 16749093 Country of ref document: EP Kind code of ref document: A1 |