WO2016056441A1 - W-ti sputtering target - Google Patents

W-ti sputtering target Download PDF

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Publication number
WO2016056441A1
WO2016056441A1 PCT/JP2015/077729 JP2015077729W WO2016056441A1 WO 2016056441 A1 WO2016056441 A1 WO 2016056441A1 JP 2015077729 W JP2015077729 W JP 2015077729W WO 2016056441 A1 WO2016056441 A1 WO 2016056441A1
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Prior art keywords
powder
concentration
mass
sputtering target
film
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PCT/JP2015/077729
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French (fr)
Japanese (ja)
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野中　荘平
齋藤　淳
健志 大友
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三菱マテリアル株式会社
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Priority to KR1020167031186A priority Critical patent/KR20160133571A/en
Priority to CN201580021546.8A priority patent/CN106460160B/en
Publication of WO2016056441A1 publication Critical patent/WO2016056441A1/en

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    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • 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
    • 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
    • C22C27/04—Alloys based on tungsten or molybdenum
    • 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

Definitions

  • the present invention relates to a W—Ti sputtering target for forming a W—Ti film as a diffusion preventing layer for preventing diffusion of mutual elements between, for example, a bump used when mounting a semiconductor element and a base electrode.
  • a W—Ti sputtering target for forming a W—Ti film as a diffusion preventing layer for preventing diffusion of mutual elements between, for example, a bump used when mounting a semiconductor element and a base electrode.
  • Au bumps, solder bumps, and the like are formed on, for example, Al electrodes and Cu electrodes.
  • Al and Au diffuse to each other to form an intermetallic compound of Al and Au, resulting in increased electrical resistance or adhesion.
  • the performance would decrease.
  • Cu electrode and the solder bump are brought into direct contact
  • Cu and Sn in the solder diffuse to each other to form an intermetallic compound of Cu and Sn, and the electrical resistance increases. There was a risk that the adhesion would be reduced.
  • a W—Ti film is formed as a diffusion preventing layer for preventing mutual element diffusion between the base electrode and the bump.
  • the W—Ti sputtering targets described in Patent Documents 1 and 2 are each manufactured by a powder sintering method.
  • Patent Document 3 discloses that by using a W—Ti sputtering target to which a small amount of Fe is added, the formed W—Ti film can contain Fe and the etching rate can be improved. .
  • Japanese Patent No. 2606946 Japanese Patent Laid-Open No. 05-295531 Japanese Patent No. 4747368
  • the etching rate is improved.
  • the Fe concentration in the W—Ti film varies, As a result, the etching rate locally changes, and uniform etching may not be performed. Therefore, a W—Ti sputtering target that can form a W—Ti film with a small variation in Fe concentration and a uniform etching rate is desired.
  • the present invention has been made in view of the above-described circumstances, and an object thereof is to provide a W—Ti sputtering target capable of forming a W—Ti film with a small variation in Fe concentration and a uniform etching rate.
  • a W—Ti sputtering target includes Ti within a range of 5 mass% to 20 mass% and Fe within a range of 25 mass ppm to 100 mass ppm.
  • W—Ti sputtering target having a composition consisting of W and the balance of inevitable impurities, the Fe concentration being measured at a plurality of locations within the target surface, and the maximum value of the measured Fe concentration being Fe max , Fe
  • the minimum value of the concentration is Fe min , (Fe max ⁇ Fe min ) / (Fe max + Fe min ) ⁇ 0.25 It is characterized by satisfying the relational expression.
  • Fe is contained in the range of 25 ppm to 100 ppm by mass, so that the etching rate of the formed W-Ti film can be increased. Can be improved. Then, the Fe concentration is measured at a plurality of locations in the target surface, and the measured maximum value of Fe concentration (Fe max ) and the minimum value of Fe concentration (Fe min ) satisfy the above relational expression, Variations in the Fe concentration in the target plane are suppressed. Therefore, it is possible to form a W—Ti film with a small variation in Fe concentration and a uniform etching rate.
  • the W-Ti sputtering target according to the present embodiment prevents diffusion between an Au bump formed on the liquid crystal driver IC and the Al pad portion (underlying electrode), for example, for bonding the liquid crystal driver IC to the COF tape. It is used when a W—Ti film is formed as a layer by sputtering.
  • the W—Ti sputtering target according to the present embodiment contains Ti in the range of 5 mass% to 20 mass%, Fe in the range of 25 mass ppm to 100 mass ppm, and the balance from W and inevitable impurities. It has the composition which becomes. Then, when the Fe concentration is measured at a plurality of locations in the target plane, the maximum value of the measured Fe concentration is Fe max , and the minimum value of the Fe concentration is Fe min , (Fe max ⁇ Fe min ) / (Fe max + Fe min ) ⁇ 0.25 And the relational expression is satisfied.
  • ⁇ Ti 5% by mass or more and 20% by mass or less>
  • the adhesion between the formed W—Ti film and the base electrode may be lowered.
  • the Ti content in the W—Ti sputtering target exceeds 20% by mass, the electrical resistance of the formed W—Ti film increases and the elements constituting the bump (in this embodiment, There is a possibility that mutual diffusion between Au) and an element constituting the base electrode (Al in this embodiment) cannot be sufficiently prevented by the formed W—Ti film.
  • the Ti content in the W—Ti sputtering target is regulated within the range of 5% by mass or more and 20% by mass or less. In addition, it is preferable to set it as 7 mass% or more, and, as for the minimum of content of Ti, it is more preferable to set it as 9 mass% or more. Further, the upper limit of the Ti content is preferably 15% by mass or less, and more preferably 13% by mass or less.
  • the Fe content in the W—Ti sputtering target is regulated within the range of 25 ppm to 100 ppm by mass.
  • the lower limit of the Fe content is preferably 30 mass ppm or more, and more preferably 35 mass ppm or more.
  • the upper limit of the Fe content is preferably 75 mass ppm or less, and more preferably 50 mass ppm or less.
  • (Fe max ⁇ Fe min ) / (Fe max + Fe min ) is preferably 0.2 or less, and more preferably 0.15 or less. Note that (Fe max -Fe min ) / (Fe max + Fe min ) is preferably as low as possible, but extremely reducing (Fe max -Fe min ) / (Fe max + Fe min ) causes an increase in cost. For this reason, (Fe max -Fe min ) / (Fe max + Fe min ) may be 0.005 or more.
  • the target surface of the W—Ti sputtering target when the target surface of the W—Ti sputtering target is circular, as shown in FIG. 2, it passes through the center (1) of the circle and the center of the circle and is orthogonal to each other.
  • the Fe concentration is measured at five points of the outer peripheral portions (2), (3), (4), and (5) on the two straight lines, and the above-mentioned maximum Fe concentration (Fe max ) and the minimum Fe concentration are measured.
  • the value (Fe min ) is obtained.
  • the outer peripheral portions (2), (3), (4), and (5) may be at a position of about 10 mm from the periphery of the target to the center side, for example. Further, when the target surface of the W—Ti sputtering target is rectangular, as shown in FIG.
  • the intersection (1) where the diagonal lines intersect and the corners (2), (3), ( 4) The Fe concentration is measured at five points (5), and the above-mentioned maximum value (Fe max ) of Fe concentration and the minimum value (Fe min ) of Fe concentration are obtained.
  • the corners (2), (3), (4), (5) may be at a position of about 10 mm from the apex to the intersection, for example.
  • the number of points where the Fe concentration is measured may be 5 or more and 20 or less. In that case, the measurement location may be a point about 10 mm from the intersection of the target center point and a straight line passing through the center and the outer periphery of the target to the center side.
  • the method for producing a W—Ti sputtering target according to the present embodiment includes a mixing and pulverizing step S01 for mixing and pulverizing the raw material powder mixed in a predetermined mixing amount, and heating the mixed and pulverized raw material powder. And a sintering step S02 for sintering and a processing step S03 for processing the obtained sintered body.
  • Ti powder, W powder and Fe powder are prepared as raw powders.
  • the W powder it is preferable to use a powder having a purity of 99.999% by mass or more and an average particle diameter of 0.5 ⁇ m or more and 20 ⁇ m or less.
  • the Fe powder it is preferable to use a powder having a purity of 99.999% by mass or more and an average particle size of 75 ⁇ m or more and 150 ⁇ m or less.
  • ⁇ Mixing and grinding step S01> These raw material powders contain Ti within a range of 5 mass% to 20 mass%, Fe within a range of 25 mass ppm to 100 mass ppm, with the balance being composed of W and inevitable impurities. While weighing, this raw material powder is mixed and pulverized. In the present embodiment, the weighed raw material powders are mixed by a ball mill, and further mixed and pulverized by an attritor device using a cemented carbide ball. By this mixing and pulverizing step S01, the Fe powder is pulverized so that the average particle diameter is 10 ⁇ m or less.
  • ⁇ Sintering step S02> the raw material powder (mixed powder) mixed and pulverized as described above is sintered in a vacuum, an inert gas atmosphere, or a reducing atmosphere.
  • the Fe powder pulverized to an average particle size of 10 ⁇ m or less is uniformly diffused in W.
  • the sintering temperature in the sintering step is preferably set according to the melting point Tm of the W—Ti alloy to be manufactured.
  • this sintering step S02 atmospheric sintering, hot pressing, or hot isostatic pressing can be applied as a sintering method.
  • the raw material powder (mixed powder) was filled in the graphite mold, and sintering was performed by vacuum hot pressing with a pressure of 10 MPa to 60 MPa and a temperature of 1000 ° C. to 1500 ° C.
  • ⁇ Processing step S03> By subjecting the sintered body obtained in the sintering step S02 to cutting or grinding, it is processed into a sputtering target having a predetermined shape.
  • the W-Ti sputtering target according to the present embodiment is manufactured through the above processes.
  • This W—Ti sputtering target is used by bonding In to a backing plate made of Cu or SUS (stainless steel) or other metal (for example, Mo) using In as a solder.
  • Fe is contained in the range of 25 ppm to 100 ppm by mass, so that the formed W—Ti film is formed.
  • the etching rate can be improved.
  • the Fe concentration is measured at a plurality of locations in the target surface, and the maximum value (Fe max ) of the measured Fe concentration and the minimum value (Fe min ) of the Fe concentration are (Fe max ⁇ Fe min ) / (Fe max + Fe min ) ⁇ 0.25 Therefore, the variation in Fe concentration in the target plane is suppressed. Therefore, it is possible to form a W—Ti film with a small variation in Fe concentration and a uniform etching rate.
  • the Ti powder, the W powder and the Fe powder are mixed and pulverized so that the particle size of the Fe powder before sintering is 10 ⁇ m or less.
  • the particle size of the Fe powder before sintering is preferably 5 ⁇ m or less, more preferably 2 ⁇ m or less, but is not limited thereto.
  • the smaller the particle size of the Fe powder before sintering the better.
  • the particle size of the Fe powder before sintering may be 0.1 ⁇ m or more.
  • Fe having an average particle diameter of 75 ⁇ m or more and 150 ⁇ m or less.
  • the powder is mixed and pulverized with other raw material powders (Ti powder, W powder) to reduce the particle size to 10 ⁇ m or less, and since the ratio of Fe powder is sufficiently low, handling becomes easy.
  • the raw powder is mixed and pulverized using an attritor device, but the present invention is not limited to this, and the raw powder may be mixed and pulverized by other methods.
  • the method for mixing and pulverizing the raw material powder include a planetary ball mill and a vibrating ball mill.
  • inevitable impurities in the W—Ti sputtering target include Na, K, Ca, Ni, Cr, and Mn. These inevitable impurities are preferably 0.01% by mass or less in total, but are not limited thereto.
  • a purity of 99.999% by mass As a raw material powder, a purity of 99.999% by mass, a Ti powder having an average particle size of 15 ⁇ m, a purity of 99.999% by mass, a W powder having an average particle size of 1 ⁇ m, a purity of 99.999% by mass, Fe powder having an average particle size of 100 ⁇ m was prepared, and Ti powder, Fe powder, and W powder were weighed so as to have the composition shown in Table 1.
  • the weighed Ti powder, Fe powder, and W powder were put into an attritor apparatus (Nippon Coke Industries, Ltd. MA1D) together with a cemented carbide ball having a diameter of about 5 mm, and the rotational speed was 300 ppm.
  • the mixed pulverization was performed for 1 hour in an Ar atmosphere under the conditions.
  • an inner paste with W foil was applied in the inside of the mixing container of this attritor.
  • the input weight of the cemented carbide ball was about 10 times the input weight of the W powder and the Fe powder.
  • the mixed and pulverized W powder, Fe powder, and Ti powder were mixed by a rolling ball mill apparatus to obtain a mixed powder.
  • the mixed powder before sintering was observed with an EPMA apparatus, Fe particles were identified by a surface analysis image of characteristic X-rays, and the particle diameter was confirmed.
  • the particle diameter is shown in Table 1. All detected Fe particles had a particle size of less than 10 ⁇ m.
  • the obtained mixed powder is filled in a graphite mold and subjected to vacuum hot pressing under conditions of pressure: 15 MPa, temperature: 1200 ° C. for 3 hours to produce a hot press sintered body, and the obtained hot press sintering is performed.
  • the body was machined to produce a W—Ti sputtering target of the present invention having a diameter of 152.4 mm and a thickness of 6 mm.
  • a purity of 99.999% by mass As a raw material powder, a purity of 99.999% by mass, a Ti powder having an average particle size of 15 ⁇ m, a purity of 99.999% by mass, a W powder having an average particle size of 1 ⁇ m, a purity of 99.999% by mass, Fe powder having an average particle size of 100 ⁇ m was prepared, and Ti powder, Fe powder, and W powder were weighed so as to have the composition shown in Table 1. The weighed Ti powder, Fe powder and W powder were mixed by a rolling ball mill device to obtain a mixed powder. That is, in the comparative example, the raw material powder was not pulverized.
  • the mixed powder before sintering was observed with an EPMA apparatus, Fe particles were identified by a surface analysis image of characteristic X-rays, and the particle diameter was confirmed.
  • the particle diameter is shown in Table 1.
  • the detected Fe particles generally had a particle diameter having a maximum value shown in Table 1.
  • the obtained mixed powder was filled in a graphite mold and subjected to vacuum hot pressing under the conditions of pressure: 15 MPa, temperature: 1200 ° C. and 3 hours to prepare a hot press sintered body.
  • the obtained hot press sintered body was machined to produce a comparative W—Ti sputtering target having a diameter of 152.4 mm and a thickness of 6 mm.
  • Substrate 100 mm diameter Si substrate ultimate vacuum: ⁇ 5 ⁇ 10 ⁇ 5 Pa Distance between substrate and target: 70mm Power: DC 600W Gas pressure: Ar 1.0Pa No substrate heating Thickness: 300nm
  • Comparative Example 1-6 As shown in Table 2, it was confirmed that the variation of the Fe concentration in the target surface was large. It is presumed that the variation in the Fe concentration in the target plane increased because sintering was performed using Fe particles having a large particle size without pulverizing the raw material powder. In particular, in Comparative Examples 2 and 5 having a low Fe concentration, the Fe concentration locally decreased, and the maximum difference in Fe concentration also increased.
  • the W—Ti sputtering target of the present invention it is possible to form a W—Ti film having a small variation in Fe concentration and a uniform etching rate.
  • the W—Ti sputtering target of the present invention forms, for example, a W—Ti film as a diffusion preventing layer for preventing diffusion of mutual elements between a bump and a base electrode used when mounting a semiconductor element. It is suitable for.

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Abstract

　This W-Ti sputtering target has a composition containing Ti in a range of 5% by mass to 20% by mass and Fe in a range of 25 ppm by mass to 100 ppm by mass, the remainder comprising W and unavoidable impurities, and satisfies the relational expression (Femax – Femin)/(Femax + Femin) ≤ 0.25, where Femax is the maximum value of the Fe concentration and Femin is the minimum value of the Fe concentration when the Fe concentration is measured in a plurality of locations in the plane of the target.

Description

Ｗ－ＴｉスパッタリングターゲットW-Ti sputtering target
　本発明は、例えば半導体素子を実装する際に用いられるバンプと下地電極との間に、相互の元素の拡散を防止する拡散防止層としてＷ－Ｔｉ膜を成膜するためのＷ－Ｔｉスパッタリングターゲットに関する。
　本願は、２０１４年１０月８日に、日本に出願された特願２０１４－２０７３４３号に基づき優先権を主張し、その内容をここに援用する。 The present invention relates to a W—Ti sputtering target for forming a W—Ti film as a diffusion preventing layer for preventing diffusion of mutual elements between, for example, a bump used when mounting a semiconductor element and a base electrode. About.
This application claims priority based on Japanese Patent Application No. 2014-207343 filed in Japan on October 8, 2014, the contents of which are incorporated herein by reference.
　従来、半導体チップを基板に実装する際には、例えばＡｌ電極やＣｕ電極の上にＡｕバンプやはんだバンプ等を形成している。
　ここで、例えばＡｌ電極とＡｕバンプとが直接接触させられた場合には、ＡｌとＡｕとが相互に拡散してＡｌとＡｕの金属間化合物が形成されてしまい、電気抵抗が上昇したり密着性が低下したりするおそれがあった。また、例えばＣｕ電極とはんだバンプとが直接接触させられた場合には、Ｃｕとはんだ中のＳｎとが相互に拡散してＣｕとＳｎの金属間化合物が形成されてしまい、電気抵抗が上昇したり密着性が低下したりするおそれがあった。 Conventionally, when a semiconductor chip is mounted on a substrate, Au bumps, solder bumps, and the like are formed on, for example, Al electrodes and Cu electrodes.
Here, for example, when an Al electrode and an Au bump are brought into direct contact, Al and Au diffuse to each other to form an intermetallic compound of Al and Au, resulting in increased electrical resistance or adhesion. There was a risk that the performance would decrease. For example, when the Cu electrode and the solder bump are brought into direct contact, Cu and Sn in the solder diffuse to each other to form an intermetallic compound of Cu and Sn, and the electrical resistance increases. There was a risk that the adhesion would be reduced.
　そこで、例えば特許文献１，２に開示されたＷ－Ｔｉスパッタリングターゲットを用いて、下地電極とバンプとの間に相互の元素の拡散を防止する拡散防止層として、Ｗ－Ｔｉ膜を形成している。
　なお、特許文献１，２に記載されたＷ－Ｔｉスパッタリングターゲットは、それぞれ粉末焼結法によって製造されている。 Therefore, for example, using a W—Ti sputtering target disclosed in Patent Documents 1 and 2, a W—Ti film is formed as a diffusion preventing layer for preventing mutual element diffusion between the base electrode and the bump. Yes.
Note that the W—Ti sputtering targets described in Patent Documents 1 and 2 are each manufactured by a powder sintering method.
　ここで、下地電極及びバンプの間に拡散防止層としてＷ－Ｔｉ膜を成膜する際には、下地電極の全面にＷ－Ｔｉ膜を成膜した上でバンプを形成し、バンプが形成されていない領域のＷ－Ｔｉ膜をエッチングで除去していた。しかし、このＷ－Ｔｉ膜は、エッチングレートが非常に遅いため、生産効率が悪いといった問題があった。
　そこで、特許文献３においては、Ｆｅを微量添加したＷ－Ｔｉスパッタリングターゲットを用いることにより、成膜されたＷ－Ｔｉ膜にＦｅを含有させ、エッチングレートを改善可能であることが開示されている。 Here, when forming a W—Ti film as a diffusion preventing layer between the base electrode and the bump, the bump is formed after forming the W—Ti film on the entire surface of the base electrode. The W—Ti film in the unexposed area was removed by etching. However, this W—Ti film has a problem that the production efficiency is poor because the etching rate is very slow.
Therefore, Patent Document 3 discloses that by using a W—Ti sputtering target to which a small amount of Fe is added, the formed W—Ti film can contain Fe and the etching rate can be improved. .
特許第２６０６９４６号公報Japanese Patent No. 2606946 特開平０５－２９５５３１号公報Japanese Patent Laid-Open No. 05-295531 特許第４７４７３６８号公報Japanese Patent No. 4747368
　ところで、上述のように、Ｗ－Ｔｉ膜にＦｅを微量添加することにより、そのエッチングレートが改善されるが、Ｗ－Ｔｉ膜においてＦｅ濃度にばらつきが生じた場合には、Ｗ－Ｔｉ膜内でエッチングレートが局所的に変化してしまい、均一なエッチングを行うことができなくなるおそれがあった。
　このため、Ｆｅ濃度のばらつきが小さくエッチングレートが均一なＷ－Ｔｉ膜を成膜することができるＷ－Ｔｉスパッタリングターゲットが望まれている。 By the way, as described above, by adding a small amount of Fe to the W—Ti film, the etching rate is improved. However, if the Fe concentration in the W—Ti film varies, As a result, the etching rate locally changes, and uniform etching may not be performed.
Therefore, a W—Ti sputtering target that can form a W—Ti film with a small variation in Fe concentration and a uniform etching rate is desired.
　この発明は、前述した事情に鑑みてなされたものであって、Ｆｅ濃度のばらつきが小さくエッチングレートが均一なＷ－Ｔｉ膜を成膜することができるＷ－Ｔｉスパッタリングターゲットを提供することを目的とする。 The present invention has been made in view of the above-described circumstances, and an object thereof is to provide a W—Ti sputtering target capable of forming a W—Ti film with a small variation in Fe concentration and a uniform etching rate. And
　上記の課題を解決するために、本発明の一態様であるＷ－Ｔｉスパッタリングターゲットは、Ｔｉを５質量％以上２０質量％以下の範囲内、Ｆｅを２５質量ｐｐｍ以上１００質量ｐｐｍ以下の範囲内で含有し、残部がＷ及び不可避不純物からなる組成を有するＷ－Ｔｉスパッタリングターゲットであって、ターゲット面内において複数個所でＦｅ濃度を測定し、測定されたＦｅ濃度の最大値をＦｅｍａｘ、Ｆｅ濃度の最小値をＦｅｍｉｎとした場合において、
　（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）≦０．２５
との関係式を満足することを特徴としている。 In order to solve the above problems, a W—Ti sputtering target according to one embodiment of the present invention includes Ti within a range of 5 mass% to 20 mass% and Fe within a range of 25 mass ppm to 100 mass ppm. W—Ti sputtering target having a composition consisting of W and the balance of inevitable impurities, the Fe concentration being measured at a plurality of locations within the target surface, and the maximum value of the measured Fe concentration being Fe max , Fe In the case where the minimum value of the concentration is Fe min ,
(Fe max −Fe min ) / (Fe max + Fe min ) ≦ 0.25
It is characterized by satisfying the relational expression.
　このような構成とされた本発明のＷ－Ｔｉスパッタリングターゲットにおいては、Ｆｅを２５質量ｐｐｍ以上１００質量ｐｐｍ以下の範囲内で含有しているので、成膜されたＷ－Ｔｉ膜のエッチングレートを改善することができる。
　そして、ターゲット面内において複数個所でＦｅ濃度を測定し、測定されたＦｅ濃度の最大値（Ｆｅｍａｘ）とＦｅ濃度の最小値（Ｆｅｍｉｎ）とが上述の関係式を満足しているので、ターゲット面内でのＦｅ濃度のばらつきが抑えられている。このため、Ｆｅ濃度のばらつきが小さくエッチングレートが均一なＷ－Ｔｉ膜を成膜することが可能となる。 In the W-Ti sputtering target of the present invention configured as described above, Fe is contained in the range of 25 ppm to 100 ppm by mass, so that the etching rate of the formed W-Ti film can be increased. Can be improved.
Then, the Fe concentration is measured at a plurality of locations in the target surface, and the measured maximum value of Fe concentration (Fe max ) and the minimum value of Fe concentration (Fe min ) satisfy the above relational expression, Variations in the Fe concentration in the target plane are suppressed. Therefore, it is possible to form a W—Ti film with a small variation in Fe concentration and a uniform etching rate.
　以上のように、本発明によれば、Ｆｅ濃度のばらつきが小さくエッチングレートが均一なＷ－Ｔｉ膜を成膜することができるＷ－Ｔｉスパッタリングターゲットを提供することが可能となる。 As described above, according to the present invention, it is possible to provide a W—Ti sputtering target capable of forming a W—Ti film with a small variation in Fe concentration and a uniform etching rate.
本発明の一実施形態に係るＷ－Ｔｉスパッタリングターゲットの製造方法を示すフロー図である。It is a flowchart which shows the manufacturing method of the W-Ti sputtering target which concerns on one Embodiment of this invention. ターゲット面が円形をなすＷ－Ｔｉスパッタリングターゲットのターゲット面におけるＦｅ濃度の測定位置を示す説明図である。It is explanatory drawing which shows the measurement position of Fe density | concentration in the target surface of the W-Ti sputtering target which makes a target surface circular. ターゲット面が矩形をなすＷ－Ｔｉスパッタリングターゲットのターゲット面におけるＦｅ濃度の測定位置を示す説明図である。It is explanatory drawing which shows the measurement position of Fe density | concentration in the target surface of the W-Ti sputtering target whose target surface forms a rectangle. 実施例において、基板上に成膜されたＷ－Ｔｉ膜のエッチングレートを測定した箇所を説明する説明図である。In an Example, it is explanatory drawing explaining the location which measured the etching rate of the W-Ti film | membrane formed into a film on the board | substrate.
　以下に、本発明の実施形態であるＷ－Ｔｉスパッタリングターゲットについて添付した図面を参照して説明する。
　本実施形態に係るＷ－Ｔｉスパッタリングターゲットは、例えば液晶ドライバーＩＣをＣＯＦテープに接合するために、液晶ドライバーＩＣ上に形成されたＡｕバンプとＡｌパッド部（下地電極）との間に、拡散防止層としてＷ－Ｔｉ膜をスパッタリングによって成膜する際に用いられる。 Hereinafter, a W—Ti sputtering target according to an embodiment of the present invention will be described with reference to the accompanying drawings.
The W-Ti sputtering target according to the present embodiment prevents diffusion between an Au bump formed on the liquid crystal driver IC and the Al pad portion (underlying electrode), for example, for bonding the liquid crystal driver IC to the COF tape. It is used when a W—Ti film is formed as a layer by sputtering.
　本実施形態に係るＷ－Ｔｉスパッタリングターゲットは、Ｔｉを５質量％以上２０質量％以下の範囲内、Ｆｅを２５質量ｐｐｍ以上１００質量ｐｐｍ以下の範囲内で含有し、残部がＷ及び不可避不純物からなる組成を有する。
　そして、ターゲット面内において複数個所でＦｅ濃度を測定し、測定されたＦｅ濃度の最大値をＦｅｍａｘ、Ｆｅ濃度の最小値をＦｅｍｉｎとした場合において、
　（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）≦０．２５
との関係式を満足している。 The W—Ti sputtering target according to the present embodiment contains Ti in the range of 5 mass% to 20 mass%, Fe in the range of 25 mass ppm to 100 mass ppm, and the balance from W and inevitable impurities. It has the composition which becomes.
Then, when the Fe concentration is measured at a plurality of locations in the target plane, the maximum value of the measured Fe concentration is Fe max , and the minimum value of the Fe concentration is Fe min ,
(Fe max −Fe min ) / (Fe max + Fe min ) ≦ 0.25
And the relational expression is satisfied.
　以下に、上述のように成分組成を規定した理由について説明する。 Hereinafter, the reason why the component composition is specified as described above will be described.
＜Ｔｉ：５質量％以上２０質量％以下＞
　Ｗ－ＴｉスパッタリングターゲットにおけるＴｉ含有量が５質量％未満とされた場合には、成膜されたＷ－Ｔｉ膜と下地電極との密着性が低下するおそれがある。一方、Ｗ－ＴｉスパッタリングターゲットにおけるＴｉ含有量が２０質量％を超えた場合には、成膜されたＷ－Ｔｉ膜の電気抵抗が上昇してしまうとともに、バンプを構成する元素（本実施形態ではＡｕ）と下地電極を構成する元素（本実施形態ではＡｌ）との相互の拡散を成膜されたＷ－Ｔｉ膜によって十分に防止できなくなるおそれがある。
　そこで、本実施形態においては、Ｗ－ＴｉスパッタリングターゲットにおけるＴｉの含有量を５質量％以上２０質量％以下の範囲内に規定している。
なお、Ｔｉの含有量の下限は、７質量％以上とすることが好ましく、９質量％以上とすることがさらに好ましい。また、Ｔｉの含有量の上限は、１５質量％以下とすることが好ましく、１３質量％以下とすることがさらに好ましい。 <Ti: 5% by mass or more and 20% by mass or less>
When the Ti content in the W—Ti sputtering target is less than 5 mass%, the adhesion between the formed W—Ti film and the base electrode may be lowered. On the other hand, when the Ti content in the W—Ti sputtering target exceeds 20% by mass, the electrical resistance of the formed W—Ti film increases and the elements constituting the bump (in this embodiment, There is a possibility that mutual diffusion between Au) and an element constituting the base electrode (Al in this embodiment) cannot be sufficiently prevented by the formed W—Ti film.
Therefore, in the present embodiment, the Ti content in the W—Ti sputtering target is regulated within the range of 5% by mass or more and 20% by mass or less.
In addition, it is preferable to set it as 7 mass% or more, and, as for the minimum of content of Ti, it is more preferable to set it as 9 mass% or more. Further, the upper limit of the Ti content is preferably 15% by mass or less, and more preferably 13% by mass or less.
＜Ｆｅ：２５質量ｐｐｍ以上１００質量ｐｐｍ以下＞
　Ｗ－ＴｉスパッタリングターゲットにおけるＦｅの含有量が２５質量ｐｐｍ未満とされた場合には、成膜されたＷ－Ｔｉ膜のエッチングレートを十分に改善することができないおそれがある。一方、Ｗ－ＴｉスパッタリングターゲットにおけるＦｅの含有量が１００質量ｐｐｍを超えた場合には、バンプを構成する元素（本実施形態ではＡｕ）と下地電極を構成する元素（本実施形態ではＡｌ）との相互の拡散を成膜されたＷ－Ｔｉ膜によって十分に防止できなくなるおそれがある。
　そこで、本実施形態においては、Ｗ－ＴｉスパッタリングターゲットにおけるＦｅの含有量を２５質量ｐｐｍ以上１００質量ｐｐｍ以下の範囲内に規定している。
　なお、Ｆｅの含有量の下限は、３０質量ｐｐｍ以上とすることが好ましく、３５質量ｐｐｍ以上とすることがさらに好ましい。また、Ｆｅの含有量の上限は、７５質量ｐｐｍ以下とすることが好ましく、５０質量ｐｐｍ以下とすることがさらに好ましい。 <Fe: 25 mass ppm or more and 100 mass ppm or less>
When the Fe content in the W—Ti sputtering target is less than 25 ppm by mass, the etching rate of the formed W—Ti film may not be sufficiently improved. On the other hand, when the Fe content in the W—Ti sputtering target exceeds 100 ppm by mass, the element constituting the bump (Au in this embodiment) and the element constituting the base electrode (Al in this embodiment) There is a possibility that the mutual diffusion of the film cannot be sufficiently prevented by the formed W—Ti film.
Therefore, in the present embodiment, the Fe content in the W—Ti sputtering target is regulated within the range of 25 ppm to 100 ppm by mass.
The lower limit of the Fe content is preferably 30 mass ppm or more, and more preferably 35 mass ppm or more. Further, the upper limit of the Fe content is preferably 75 mass ppm or less, and more preferably 50 mass ppm or less.
＜（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）≦０．２５＞
　本実施形態におけるＷ－Ｔｉスパッタリングターゲットを用いてＷ－Ｔｉ膜を成膜する場合には、Ｗ－Ｔｉスパッタリングターゲットのターゲット面の全体からそれぞれ原子がはじき飛ばされて成膜される。
　ここで、ターゲット面内において複数個所でＦｅ濃度を測定し、測定されたＦｅ濃度の最大値（Ｆｅｍａｘ）とＦｅ濃度の最小値（Ｆｅｍｉｎ）とが上述の関係式を満足する場合には、ターゲット面内においてＦｅ濃度のばらつきが小さくなる。よって、このＷ－Ｔｉスパッタリングターゲットを用いて成膜したＷ－Ｔｉ膜においても、Ｆｅ濃度のばらつきが小さくなり、エッチングレートが均一となる。
　なお、（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）は、０．２以下とすることが好ましく、０．１５以下とすることがさらに好ましい。なお（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）は低いほど好ましいが、（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）を極度に低下させることはコストの増加を招く。このため、（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）は０．００５以上であってもよい。 <(Fe max −Fe min ) / (Fe max + Fe min ) ≦ 0.25>
When a W—Ti film is formed using the W—Ti sputtering target in this embodiment, atoms are repelled from the entire target surface of the W—Ti sputtering target.
Here, when the Fe concentration is measured at a plurality of locations in the target surface, and the measured maximum value of Fe concentration (Fe max ) and the minimum value of Fe concentration (Fe min ) satisfy the above relational expression, In the target surface, the variation in Fe concentration is reduced. Therefore, even in a W—Ti film formed using this W—Ti sputtering target, the variation in Fe concentration becomes small and the etching rate becomes uniform.
Note that (Fe max −Fe min ) / (Fe max + Fe min ) is preferably 0.2 or less, and more preferably 0.15 or less. Note that (Fe max -Fe min ) / (Fe max + Fe min ) is preferably as low as possible, but extremely reducing (Fe max -Fe min ) / (Fe max + Fe min ) causes an increase in cost. For this reason, (Fe max -Fe min ) / (Fe max + Fe min ) may be 0.005 or more.
　ここで、本実施形態においては、Ｗ－Ｔｉスパッタリングターゲットのターゲット面が円形をなす場合には、図２に示すように、円の中心（１）、及び、円の中心を通過するとともに互いに直交する２本の直線上の外周部分（２）、（３）、（４）、（５）の５点でＦｅ濃度を測定し、上述のＦｅ濃度の最大値（Ｆｅｍａｘ）とＦｅ濃度の最小値（Ｆｅｍｉｎ）を求めている。外周部分（２）、（３）、（４）、（５）は、例えばターゲットの周縁から中心側に約１０ｍｍの位置であってもよい。
　また、Ｗ－Ｔｉスパッタリングターゲットのターゲット面が矩形をなす場合には、図３に示すように、対角線が交差する交点（１）と、各対角線上の角部（２）、（３）、（４）、（５）の５点でＦｅ濃度を測定し、上述のＦｅ濃度の最大値（Ｆｅｍａｘ）とＦｅ濃度の最小値（Ｆｅｍｉｎ）を求めている。角部（２）、（３）、（４）、（５）は、例えば頂点から交点側に約１０ｍｍの位置であってもよい。
　Ｆｅ濃度の測定箇所の数は、５点以上２０点以下であってもよい。その場合、測定箇所は、ターゲット中心点と、その中心を通る直線とターゲット外周縁との交点から中心側に約１０ｍｍの点であってもよい。 Here, in the present embodiment, when the target surface of the W—Ti sputtering target is circular, as shown in FIG. 2, it passes through the center (1) of the circle and the center of the circle and is orthogonal to each other. The Fe concentration is measured at five points of the outer peripheral portions (2), (3), (4), and (5) on the two straight lines, and the above-mentioned maximum Fe concentration (Fe max ) and the minimum Fe concentration are measured. The value (Fe min ) is obtained. The outer peripheral portions (2), (3), (4), and (5) may be at a position of about 10 mm from the periphery of the target to the center side, for example.
Further, when the target surface of the W—Ti sputtering target is rectangular, as shown in FIG. 3, the intersection (1) where the diagonal lines intersect and the corners (2), (3), ( 4) The Fe concentration is measured at five points (5), and the above-mentioned maximum value (Fe max ) of Fe concentration and the minimum value (Fe min ) of Fe concentration are obtained. The corners (2), (3), (4), (5) may be at a position of about 10 mm from the apex to the intersection, for example.
The number of points where the Fe concentration is measured may be 5 or more and 20 or less. In that case, the measurement location may be a point about 10 mm from the intersection of the target center point and a straight line passing through the center and the outer periphery of the target to the center side.
　次に、本実施形態に係るＷ－Ｔｉスパッタリングターゲットを製造する一実施形態について、図１のフロー図を参照して説明する。
　本実施形態に係るＷ－Ｔｉスパッタリングターゲットの製造方法は、図１に示すように、所定の配合量で配合された原料粉を混合粉砕する混合粉砕工程Ｓ０１と、混合粉砕された原料粉を加熱して焼結させる焼結工程Ｓ０２と、得られた焼結体を加工する加工工程Ｓ０３と、を備えている。 Next, an embodiment for producing a W—Ti sputtering target according to this embodiment will be described with reference to the flowchart of FIG.
As shown in FIG. 1, the method for producing a W—Ti sputtering target according to the present embodiment includes a mixing and pulverizing step S01 for mixing and pulverizing the raw material powder mixed in a predetermined mixing amount, and heating the mixed and pulverized raw material powder. And a sintering step S02 for sintering and a processing step S03 for processing the obtained sintered body.
　まず、原料粉として、Ｔｉ粉末、Ｗ粉末及びＦｅ粉末を準備する。ここで、Ｔｉ粉末としては、純度が９９．９９９質量％以上、平均粒径が１μｍ以上４０μｍ以下とされたものを用いることが好ましい。また、Ｗ粉末としては、純度が９９．９９９質量％以上、平均粒径が０．５μｍ以上２０μｍ以下とされたものを用いることが好ましい。さらに、Ｆｅ粉末としては、純度が９９．９９９質量％以上、平均粒径が７５μｍ以上１５０μｍ以下とされたものを用いることが好ましい。 First, Ti powder, W powder and Fe powder are prepared as raw powders. Here, it is preferable to use a Ti powder having a purity of 99.999 mass% or more and an average particle diameter of 1 μm or more and 40 μm or less. Further, as the W powder, it is preferable to use a powder having a purity of 99.999% by mass or more and an average particle diameter of 0.5 μm or more and 20 μm or less. Further, as the Fe powder, it is preferable to use a powder having a purity of 99.999% by mass or more and an average particle size of 75 μm or more and 150 μm or less.
＜混合粉砕工程Ｓ０１＞
　これらの原料粉を、Ｔｉを５質量％以上２０質量％以下の範囲内、Ｆｅを２５質量ｐｐｍ以上１００質量ｐｐｍ以下の範囲内で含有し、残部がＷ及び不可避不純物からなる組成となるように秤量するとともに、この原料粉を混合粉砕する。本実施形態においては、秤量された原料粉をボールミルによって混合し、さらに超硬合金製のボールを用いて、アトライタ装置によって混合粉砕する。
　この混合粉砕工程Ｓ０１により、Ｆｅ粉末は、平均粒径が１０μｍ以下になるように粉砕される。 <Mixing and grinding step S01>
These raw material powders contain Ti within a range of 5 mass% to 20 mass%, Fe within a range of 25 mass ppm to 100 mass ppm, with the balance being composed of W and inevitable impurities. While weighing, this raw material powder is mixed and pulverized. In the present embodiment, the weighed raw material powders are mixed by a ball mill, and further mixed and pulverized by an attritor device using a cemented carbide ball.
By this mixing and pulverizing step S01, the Fe powder is pulverized so that the average particle diameter is 10 μm or less.
＜焼結工程Ｓ０２＞
　次に、上述のようにして混合粉砕された原料粉（混合粉）を、真空又は不活性ガス雰囲気中又は還元雰囲気中で焼結を行う。この焼結工程Ｓ０２において、平均粒径が１０μｍ以下にまで粉砕されたＦｅ粉末は、Ｗ中に均一に拡散される。
　ここで、焼結工程における焼結温度は、製造するＷ－Ｔｉ合金の融点Ｔｍに応じて設定することが好ましい。 <Sintering step S02>
Next, the raw material powder (mixed powder) mixed and pulverized as described above is sintered in a vacuum, an inert gas atmosphere, or a reducing atmosphere. In this sintering step S02, the Fe powder pulverized to an average particle size of 10 μm or less is uniformly diffused in W.
Here, the sintering temperature in the sintering step is preferably set according to the melting point Tm of the W—Ti alloy to be manufactured.
　この焼結工程Ｓ０２において、焼結方法として、常圧焼結、ホットプレス、熱間静水圧プレスを適用することが可能である。
　本実施形態では、グラファイト製モールドに原料粉（混合粉）を充填し、圧力を１０ＭＰａ以上６０ＭＰａ以下、温度を１０００℃以上１５００℃、とした真空ホットプレスによって焼結を行った。 In this sintering step S02, atmospheric sintering, hot pressing, or hot isostatic pressing can be applied as a sintering method.
In this embodiment, the raw material powder (mixed powder) was filled in the graphite mold, and sintering was performed by vacuum hot pressing with a pressure of 10 MPa to 60 MPa and a temperature of 1000 ° C. to 1500 ° C.
＜加工工程Ｓ０３＞
　焼結工程Ｓ０２で得られた焼結体に対して切削加工又は研削加工を施すことにより、所定形状のスパッタリングターゲットに加工する。 <Processing step S03>
By subjecting the sintered body obtained in the sintering step S02 to cutting or grinding, it is processed into a sputtering target having a predetermined shape.
　以上のような工程により、本実施形態であるＷ－Ｔｉスパッタリングターゲットが製造される。このＷ－Ｔｉスパッタリングターゲットは、Ｉｎをはんだとして、Ｃｕ又はＳＵＳ（ステンレス）又はその他の金属（例えばＭｏ）からなるバッキングプレートにボンディングして使用される。 The W-Ti sputtering target according to the present embodiment is manufactured through the above processes. This W—Ti sputtering target is used by bonding In to a backing plate made of Cu or SUS (stainless steel) or other metal (for example, Mo) using In as a solder.
　以上のような構成とされた本実施形態であるＷ－Ｔｉスパッタリングターゲットによれば、Ｆｅを２５質量ｐｐｍ以上１００質量ｐｐｍ以下の範囲内で含有しているので、成膜されたＷ－Ｔｉ膜のエッチングレートを改善することができる。
　そして、ターゲット面内において複数個所でＦｅ濃度を測定し、測定されたＦｅ濃度の最大値（Ｆｅｍａｘ）とＦｅ濃度の最小値（Ｆｅｍｉｎ）とが、
　（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）≦０．２５
の関係式を満足しているので、ターゲット面内でのＦｅ濃度のばらつきが抑えられている。よって、Ｆｅ濃度のばらつきが小さくエッチングレートが均一なＷ－Ｔｉ膜を成膜することが可能となる。 According to the W—Ti sputtering target of the present embodiment configured as described above, Fe is contained in the range of 25 ppm to 100 ppm by mass, so that the formed W—Ti film is formed. The etching rate can be improved.
Then, the Fe concentration is measured at a plurality of locations in the target surface, and the maximum value (Fe max ) of the measured Fe concentration and the minimum value (Fe min ) of the Fe concentration are
(Fe max −Fe min ) / (Fe max + Fe min ) ≦ 0.25
Therefore, the variation in Fe concentration in the target plane is suppressed. Therefore, it is possible to form a W—Ti film with a small variation in Fe concentration and a uniform etching rate.
　また、本実施形態では、Ｔｉ粉末、Ｗ粉末及びＦｅ粉末を混合粉砕することにより、焼結前のＦｅ粉末の粒径が１０μｍ以下とされているので、焼結時において、Ｆｅ粒子を母相となるＷ中に均一に拡散させることができ、焼結体全体にＦｅを均一に分布させることが可能となる。焼結前のＦｅ粉末の粒径は、５μｍ以下が好ましく、２μｍ以下がさらに好ましいが、これに限定されることはない。また、焼結前のＦｅ粉末の粒径は小さいほど好ましいが、焼結前のＦｅ粉末の粒径を極度に低下させることはコストの増加を招く。このため、焼結前のＦｅ粉末の粒径は０．１μｍ以上であってもよい。
　なお、５０μｍ以下の粒子を全体の５０％以上含む微細なＦｅ粉末を直接使用した場合には危険物として取り扱う必要があるが、本実施形態では、平均粒径が７５μｍ以上１５０μｍ以下とされたＦｅ粉末を、他の原料粉（Ｔｉ粉末、Ｗ粉末）とともに混合粉砕することで粒径を１０μｍ以下としており、さらにＦｅ粉末の比率が十分に低いことから、取り扱いが容易となる。 In this embodiment, the Ti powder, the W powder and the Fe powder are mixed and pulverized so that the particle size of the Fe powder before sintering is 10 μm or less. Thus, it is possible to diffuse uniformly in W, and to uniformly distribute Fe throughout the sintered body. The particle size of the Fe powder before sintering is preferably 5 μm or less, more preferably 2 μm or less, but is not limited thereto. In addition, the smaller the particle size of the Fe powder before sintering, the better. However, extremely reducing the particle size of the Fe powder before sintering causes an increase in cost. For this reason, the particle size of the Fe powder before sintering may be 0.1 μm or more.
In addition, when fine Fe powder containing 50% or more of particles of 50 μm or less is directly used, it is necessary to handle it as a dangerous substance, but in this embodiment, Fe having an average particle diameter of 75 μm or more and 150 μm or less. The powder is mixed and pulverized with other raw material powders (Ti powder, W powder) to reduce the particle size to 10 μm or less, and since the ratio of Fe powder is sufficiently low, handling becomes easy.
　以上、本発明の実施形態について説明したが、本発明はこれに限定されることはなく、その発明の技術的思想を逸脱しない範囲で適宜変更可能である。
　例えば、本実施形態では、アトライタ装置を用いて原料粉を混合粉砕するものとして説明したが、これに限定されることはなく、他の方法によって原料粉を混合粉砕してもよい。
　なお、原料粉を混合粉砕する方法としては、遊星ボールミル、振動ボールミル等が挙げられる。
　Ｗ－Ｔｉスパッタリングターゲットにおける不可避不純物としては、Ｎａ、Ｋ、Ｃａ、Ｎｉ、Ｃｒ、Ｍｎ等が挙げられる。これらの不可避不純物は、合計で０．０１質量％以下であることが好ましいが、これに限定されることはない。 As mentioned above, although embodiment of this invention was described, this invention is not limited to this, It can change suitably in the range which does not deviate from the technical idea of the invention.
For example, in the present embodiment, the raw powder is mixed and pulverized using an attritor device, but the present invention is not limited to this, and the raw powder may be mixed and pulverized by other methods.
Examples of the method for mixing and pulverizing the raw material powder include a planetary ball mill and a vibrating ball mill.
Examples of inevitable impurities in the W—Ti sputtering target include Na, K, Ca, Ni, Cr, and Mn. These inevitable impurities are preferably 0.01% by mass or less in total, but are not limited thereto.
　以下に、本発明に係るＷ－Ｔｉスパッタリングターゲットの作用効果について評価した評価試験の結果について説明する。 Hereinafter, the results of an evaluation test for evaluating the function and effect of the W—Ti sputtering target according to the present invention will be described.
＜本発明例＞
　原料粉末として、純度が９９．９９９質量％、平均粒径が１５μｍとされたＴｉ粉末、純度が９９．９９９質量％、平均粒径が１μｍとされたＷ粉末、純度が９９．９９９質量％、平均粒径が１００μｍとされたＦｅ粉末を用意し、表１に示す組成となるように、Ｔｉ粉末、Ｆｅ粉末及びＷ粉末を秤量した。 <Invention Example>
As a raw material powder, a purity of 99.999% by mass, a Ti powder having an average particle size of 15 μm, a purity of 99.999% by mass, a W powder having an average particle size of 1 μm, a purity of 99.999% by mass, Fe powder having an average particle size of 100 μm was prepared, and Ti powder, Fe powder, and W powder were weighed so as to have the composition shown in Table 1.
　秤量されたＴｉ粉末、Ｆｅ粉末及びＷ粉末のうち、Ｗ粉末とＦｅ粉末をアトライタ装置（日本コークス工業株式会社ＭＡ１Ｄ）に、直径約５ｍｍの超硬合金製ボールととともに投入し、回転数３００ｐｐｍの条件にてＡｒ雰囲気下で１時間の混合粉砕を実施した。なお、このアトライタの混合容器の内側には、粉砕混合時の容器からの不純物の混入を防止するため、Ｗ箔による内貼りを施した。ここで、超硬合金製ボールの投入重量は、Ｗ粉末とＦｅ粉末の投入重量の約１０倍とした。 Of the weighed Ti powder, Fe powder, and W powder, W powder and Fe powder were put into an attritor apparatus (Nippon Coke Industries, Ltd. MA1D) together with a cemented carbide ball having a diameter of about 5 mm, and the rotational speed was 300 ppm. The mixed pulverization was performed for 1 hour in an Ar atmosphere under the conditions. In addition, in the inside of the mixing container of this attritor, in order to prevent mixing of impurities from the container at the time of pulverization and mixing, an inner paste with W foil was applied. Here, the input weight of the cemented carbide ball was about 10 times the input weight of the W powder and the Fe powder.
　混合粉砕されたＷ粉末及びＦｅ粉末、並びに、Ｔｉ粉末を、転動ボールミル装置によって混合し、混合粉末を得た。ここで、焼結前の混合粉末をＥＰＭＡ装置にて観察し、特性Ｘ線の面分析像によりＦｅ粒子を特定し、その粒子径を確認した。その粒子径を表１に示す。検出されたＦｅ粒子は全て１０μｍ未満の粒子径を有していた。 The mixed and pulverized W powder, Fe powder, and Ti powder were mixed by a rolling ball mill apparatus to obtain a mixed powder. Here, the mixed powder before sintering was observed with an EPMA apparatus, Fe particles were identified by a surface analysis image of characteristic X-rays, and the particle diameter was confirmed. The particle diameter is shown in Table 1. All detected Fe particles had a particle size of less than 10 μm.
　得られた混合粉末をグラファイト製モールドに充填し、圧力：１５ＭＰａ、温度：１２００℃、３時間保持の条件で真空ホットプレスすることによりホットプレス焼結体を作製し、得られたホットプレス焼結体を機械加工して直径：１５２．４ｍｍ、厚さ：６ｍｍを有する本発明例のＷ－Ｔｉスパッタリングターゲットを作製した。 The obtained mixed powder is filled in a graphite mold and subjected to vacuum hot pressing under conditions of pressure: 15 MPa, temperature: 1200 ° C. for 3 hours to produce a hot press sintered body, and the obtained hot press sintering is performed. The body was machined to produce a W—Ti sputtering target of the present invention having a diameter of 152.4 mm and a thickness of 6 mm.
＜比較例＞
　原料粉末として、純度が９９．９９９質量％、平均粒径が１５μｍとされたＴｉ粉末、純度が９９．９９９質量％、平均粒径が１μｍとされたＷ粉末、純度が９９．９９９質量％、平均粒径が１００μｍとされたＦｅ粉末を用意し、表１に示す組成となるように、Ｔｉ粉末、Ｆｅ粉末及びＷ粉末を秤量した。
　秤量されたＴｉ粉末、Ｆｅ粉末及びＷ粉末を転動ボールミル装置によって混合し、混合粉末を得た。すなわち、比較例では、原料粉の粉砕を実施しなかった。ここで、焼結前の混合粉末をＥＰＭＡ装置にて観察し、特性Ｘ線の面分析像によりＦｅ粒子を特定し、その粒子径を確認した。その粒子径を表１に示す。検出されたＦｅ粒子は概ね表１に示す値を最大値とする粒子径を有していた。 <Comparative example>
As a raw material powder, a purity of 99.999% by mass, a Ti powder having an average particle size of 15 μm, a purity of 99.999% by mass, a W powder having an average particle size of 1 μm, a purity of 99.999% by mass, Fe powder having an average particle size of 100 μm was prepared, and Ti powder, Fe powder, and W powder were weighed so as to have the composition shown in Table 1.
The weighed Ti powder, Fe powder and W powder were mixed by a rolling ball mill device to obtain a mixed powder. That is, in the comparative example, the raw material powder was not pulverized. Here, the mixed powder before sintering was observed with an EPMA apparatus, Fe particles were identified by a surface analysis image of characteristic X-rays, and the particle diameter was confirmed. The particle diameter is shown in Table 1. The detected Fe particles generally had a particle diameter having a maximum value shown in Table 1.
　得られた混合粉末をグラファイト製モールドに充填し、圧力：１５ＭＰａ、温度：１２００℃、３時間保持の条件で真空ホットプレスすることによりホットプレス焼結体を作製した。得られたホットプレス焼結体を機械加工して直径：１５２．４ｍｍ、厚さ：６ｍｍを有する比較例のＷ－Ｔｉスパッタリングターゲットを作製した。 The obtained mixed powder was filled in a graphite mold and subjected to vacuum hot pressing under the conditions of pressure: 15 MPa, temperature: 1200 ° C. and 3 hours to prepare a hot press sintered body. The obtained hot press sintered body was machined to produce a comparative W—Ti sputtering target having a diameter of 152.4 mm and a thickness of 6 mm.
＜ターゲット面内のＦｅ濃度＞
　得られたＷ－Ｔｉスパッタリングターゲットのターゲット面が円形（丸型ターゲット）である場合には、図２に示すように、円の中心（１）と、中心を通過するとともに互いに直交する２本の直線上の外周から約１０ｍｍの位置（２）、（３）、（４）、（５）の５点から、超硬合金製のドリルを用いて組成分析用の試料を採取した。
　また、得られたＷ－Ｔｉスパッタリングターゲットのターゲット面が矩形（角型ターゲット）である場合には、図３に示すように、対角線が交差する交点（１）と、各対角線上の角部から約１０ｍｍの位置（２）、（３）、（４）、（５）の５点から、超硬合金製のドリルを用いて組成分析用の試料を採取した。
　これらの試料のＦｅ濃度をＩＣＰ発光分光分析法により分析した。測定結果を表２に示す。 <Fe concentration in the target surface>
When the target surface of the obtained W—Ti sputtering target is circular (round target), as shown in FIG. 2, the center (1) of the circle and the two passing through the center and orthogonal to each other Samples for composition analysis were collected from 5 points of positions (2), (3), (4), and (5) about 10 mm from the outer periphery on a straight line using a drill made of cemented carbide.
In addition, when the target surface of the obtained W—Ti sputtering target is a rectangle (square target), as shown in FIG. 3, from the intersection (1) where the diagonal lines intersect and the corners on each diagonal line Samples for composition analysis were collected from 5 points of positions (2), (3), (4), and (5) of about 10 mm using a drill made of cemented carbide.
The Fe concentration of these samples was analyzed by ICP emission spectroscopy. The measurement results are shown in Table 2.
＜Ｗ－Ｔｉ膜の成膜＞
　次に、上述の本発明例及び比較例のＷ－Ｔｉスパッタリングターゲットを無酸素銅製のバッキングプレートにはんだ付けし、これをスパッタ装置（株式会社アルバック製ＳＩＨ－４５０Ｈ）に装着し、以下の条件にてスパッタリング成膜を実施した。 <Deposition of W-Ti film>
Next, the W-Ti sputtering targets of the above-described inventive examples and comparative examples are soldered to a backing plate made of oxygen-free copper, and this is mounted on a sputtering apparatus (SIH-450H manufactured by ULVAC, Inc.). Then, sputtering film formation was performed.
基板：直径１００ｍｍのＳｉ基板
到達真空度：＜５×１０－５Ｐａ
基板とターゲットの距離：７０ｍｍ
電力：直流６００Ｗ
ガス圧力：　Ａｒ　１．０Ｐａ
基板加熱　なし
膜厚：３００ｎｍ Substrate: 100 mm diameter Si substrate ultimate vacuum: <5 × 10 −5 Pa
Distance between substrate and target: 70mm
Power: DC 600W
Gas pressure: Ar 1.0Pa
No substrate heating Thickness: 300nm
＜Ｗ－Ｔｉ膜のエッチングレート評価＞
　このようにして得られた直径１００ｍｍのＳｉ基板のうち図４に示す３箇所の位置から、２０ｍｍ角の試料を切り出した。さらにこの試料を、１０ｍｍ×２０ｍｍの二つの部分に切断し、切断した片方の試料をウォーターバスにより液温３０℃に設定された３１ｖｏｌ％過酸化水素水に５分間浸漬した。過酸化水素から取り出した後、純水で十分すすぎ、さらに付着した純水の液滴を、乾燥空気を吹き付けて飛ばし、試料を乾燥させた。 <Evaluation of etching rate of W-Ti film>
A 20 mm square sample was cut out from three positions shown in FIG. 4 in the Si substrate having a diameter of 100 mm obtained in this manner. Further, this sample was cut into two parts of 10 mm × 20 mm, and one of the cut samples was immersed in a 31 vol% hydrogen peroxide solution set at a liquid temperature of 30 ° C. for 5 minutes by a water bath. After removing from the hydrogen peroxide, the sample was sufficiently rinsed with pure water, and the adhered pure water droplets were blown off with dry air to dry the sample.
　この試料の過酸化水素水に浸漬していない側と、浸漬した側の両方について断面をフィールドエミッション式の走査電子顕微鏡（ＦＥ－ＳＥＭ：株式会社日立ハイテクノロジーズ製ＳＵ－７０）にて観察し、Ｗ－Ｔｉ膜の膜厚を測定した。過酸化水素に浸漬した側としていない側の膜厚差を求め、この膜厚差を浸漬時間（５分）で割り、直径１００ｍｍの基板の各位置におけるエッチングレートを算出した。この結果を表３に示す。 The cross section of both the side not immersed in the hydrogen peroxide solution and the immersed side of this sample was observed with a field emission type scanning electron microscope (FE-SEM: SU-70 manufactured by Hitachi High-Technologies Corporation). The film thickness of the W—Ti film was measured. The difference in film thickness on the side not immersed in hydrogen peroxide was determined, and the difference in film thickness was divided by the immersion time (5 minutes) to calculate the etching rate at each position of the substrate having a diameter of 100 mm. The results are shown in Table 3.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
　比較例１－６においては、表２に示すように、ターゲット面内におけるＦｅ濃度のばらつきが大きくなっていることが確認された。ターゲット面内におけるＦｅ濃度のばらつきが大きくなったのは、原料粉の粉砕を行わずに、粒径の大きなＦｅ粒子を用いて焼結を行ったためと推測される。
　特に、Ｆｅ濃度の低い比較例２、５では、Ｆｅ濃度が局所的に少なくなっており、Ｆｅ濃度の最大差も大きくなっていた。 In Comparative Example 1-6, as shown in Table 2, it was confirmed that the variation of the Fe concentration in the target surface was large. It is presumed that the variation in the Fe concentration in the target plane increased because sintering was performed using Fe particles having a large particle size without pulverizing the raw material powder.
In particular, in Comparative Examples 2 and 5 having a low Fe concentration, the Fe concentration locally decreased, and the maximum difference in Fe concentration also increased.
　この比較例１－６のＷ－Ｔｉスパッタリングターゲットを用いて成膜された比較例１１－１６のＷ－Ｔｉ膜においては、エッチングレートが不均一であることが確認された。
　また、Ｆｅ濃度の低い比較例２、５のＷ－Ｔｉスパッタリングターゲットを用いて成膜された比較例１２、１５のＷ－Ｔｉ膜においては、局所的にエッチングレートが非常に遅くなっていることが確認された。 It was confirmed that the etching rate was nonuniform in the W—Ti film of Comparative Example 11-16 formed using the W—Ti sputtering target of Comparative Example 1-6.
In addition, in the W—Ti films of Comparative Examples 12 and 15 formed using the W—Ti sputtering targets of Comparative Examples 2 and 5 having a low Fe concentration, the etching rate is extremely slow locally. Was confirmed.
　これに対して、本発明例１－６においては、ターゲット面内におけるＦｅ濃度のばらつきが小さくなっていることが確認された。ターゲット面内におけるＦｅ濃度のばらつきが小さくなったのは、原料粉の混合粉砕を行うことで、粒径の小さなＦｅ粒子を用いて焼結を行ったためと推測される。
　また、Ｆｅ濃度の低い本発明例２、５やＦｅ濃度の高い本発明例３、６においても、Ｆｅ濃度のばらつきが小さく安定していた。 On the other hand, in Inventive Example 1-6, it was confirmed that the variation in Fe concentration in the target plane was small. The reason why the variation in the Fe concentration in the target surface is small is presumed that the raw powder was mixed and pulverized to sinter using Fe particles having a small particle size.
Further, in Invention Examples 2 and 5 having a low Fe concentration and Invention Examples 3 and 6 having a high Fe concentration, the variation in Fe concentration was small and stable.
　この本発明例１－６のＷ－Ｔｉスパッタリングターゲットを用いて成膜された本発明例１１－１６のＷ－Ｔｉ膜においては、エッチングレートが均一であることが確認された。
　特に、Ｆｅ濃度の低い本発明例２、５のＷ－Ｔｉスパッタリングターゲットを用いて成膜された本発明例１２、１５のＷ－Ｔｉ膜においても、Ｗ－Ｔｉ膜に確実にＦｅが添加されており、エッチングレートが安定していた。
　また、Ｆｅ濃度が高い本発明例３、６のＷ－Ｔｉスパッタリングターゲットを用いて成膜された本発明例１３、１６のＷ－Ｔｉ膜においても、エッチングレートのばらつきが十分に抑えられていた。 In the W—Ti film of Invention Example 11-16 formed using the W—Ti sputtering target of Invention Example 1-6, it was confirmed that the etching rate was uniform.
In particular, even in the W—Ti films of Invention Examples 12 and 15 formed using the W—Ti sputtering targets of Invention Examples 2 and 5 having a low Fe concentration, Fe was reliably added to the W—Ti film. The etching rate was stable.
In addition, in the W—Ti films of Invention Examples 13 and 16 formed using the W—Ti sputtering target of Invention Examples 3 and 6 having a high Fe concentration, the variation in etching rate was sufficiently suppressed. .
　以上の確認実験の結果から、本発明例によれば、Ｆｅ濃度のばらつきが小さくエッチングレートが均一なＷ－Ｔｉ膜を成膜することができることが確認された。 From the results of the above confirmation experiment, it was confirmed that according to the example of the present invention, it is possible to form a W—Ti film having a small variation in Fe concentration and a uniform etching rate.
　本発明のＷ－Ｔｉスパッタリングターゲットによれば、Ｆｅ濃度のばらつきが小さくエッチングレートが均一なＷ－Ｔｉ膜を成膜することが可能である。本発明のＷ－Ｔｉスパッタリングターゲットは、例えば半導体素子を実装する際に用いられるバンプと下地電極との間に、相互の元素の拡散を防止する拡散防止層としてのＷ－Ｔｉ膜を成膜するのに好適である。 According to the W—Ti sputtering target of the present invention, it is possible to form a W—Ti film having a small variation in Fe concentration and a uniform etching rate. The W—Ti sputtering target of the present invention forms, for example, a W—Ti film as a diffusion preventing layer for preventing diffusion of mutual elements between a bump and a base electrode used when mounting a semiconductor element. It is suitable for.

Claims (1)

  1. 　Ｔｉを５質量％以上２０質量％以下の範囲内、Ｆｅを２５質量ｐｐｍ以上１００質量ｐｐｍ以下の範囲内で含有し、残部がＷ及び不可避不純物からなる組成を有するＷ－Ｔｉスパッタリングターゲットであって、
    　ターゲット面内において複数個所でＦｅ濃度を測定し、測定されたＦｅ濃度の最大値をＦｅｍａｘ、Ｆｅ濃度の最小値をＦｅｍｉｎとした場合において、
    　（Ｆｅｍａｘ－Ｆｅｍｉｎ）／（Ｆｅｍａｘ＋Ｆｅｍｉｎ）≦０．２５
    との関係式を満足するＷ－Ｔｉスパッタリングターゲット。     A W—Ti sputtering target containing Ti in a range of 5 mass% to 20 mass%, Fe in a range of 25 mass ppm to 100 mass ppm, with the balance being composed of W and inevitable impurities. ,
    When the Fe concentration is measured at a plurality of locations in the target plane, the maximum value of the measured Fe concentration is Fe max , and the minimum value of the Fe concentration is Fe min ,
    (Fe max −Fe min ) / (Fe max + Fe min ) ≦ 0.25
    W-Ti sputtering target satisfying the relational expression
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020095595A1 (en) * 2018-11-06 2020-05-14 三菱マテリアル株式会社 W-Ti SPUTTERING TARGET

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111155061A (en) * 2018-11-07 2020-05-15 宁波江丰电子材料股份有限公司 Preparation method of WTi alloy target
CN112111713B (en) * 2020-09-11 2022-09-30 宁波江丰电子材料股份有限公司 Preparation method of WTi alloy sputtering target material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03264640A (en) * 1990-03-13 1991-11-25 Hitachi Metals Ltd Ti-w target material and production thereof
JPH05295531A (en) * 1992-04-21 1993-11-09 Toshiba Corp Ti-w based sputtering target and its production
JP2008218693A (en) * 2007-03-05 2008-09-18 Mitsubishi Materials Corp W-Ti DIFFUSION-PREVENTING FILM HAVING HIGH ETCHING RATE, AND W-Ti TARGET FOR SPUTTERING FOR FORMING THE SAME
WO2013175884A1 (en) * 2012-05-22 2013-11-28 Jx日鉱日石金属株式会社 Fe-Pt-Ag-C-BASED SPUTTERING TARGET HAVING C PARTICLES DISPERSED THEREIN, AND METHOD FOR PRODUCING SAME
WO2014148588A1 (en) * 2013-03-22 2014-09-25 Jx日鉱日石金属株式会社 Tungsten-sintered-body sputtering target and method for producing same

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5156591B2 (en) * 2008-11-17 2013-03-06 出光興産株式会社 Organic electroluminescence device
JP2011058078A (en) * 2009-09-14 2011-03-24 Toshiba Corp SPUTTERING TARGET, Ta-W ALLOY FILM USING THE SAME, AND LIQUID CRYSTAL DISPLAY DEVICE

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03264640A (en) * 1990-03-13 1991-11-25 Hitachi Metals Ltd Ti-w target material and production thereof
JPH05295531A (en) * 1992-04-21 1993-11-09 Toshiba Corp Ti-w based sputtering target and its production
JP2008218693A (en) * 2007-03-05 2008-09-18 Mitsubishi Materials Corp W-Ti DIFFUSION-PREVENTING FILM HAVING HIGH ETCHING RATE, AND W-Ti TARGET FOR SPUTTERING FOR FORMING THE SAME
WO2013175884A1 (en) * 2012-05-22 2013-11-28 Jx日鉱日石金属株式会社 Fe-Pt-Ag-C-BASED SPUTTERING TARGET HAVING C PARTICLES DISPERSED THEREIN, AND METHOD FOR PRODUCING SAME
WO2014148588A1 (en) * 2013-03-22 2014-09-25 Jx日鉱日石金属株式会社 Tungsten-sintered-body sputtering target and method for producing same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020095595A1 (en) * 2018-11-06 2020-05-14 三菱マテリアル株式会社 W-Ti SPUTTERING TARGET

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CN106460160B (en) 2018-08-17

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