WO2022045196A1 - Cible de pulvérisation - Google Patents

Cible de pulvérisation Download PDF

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Publication number
WO2022045196A1
WO2022045196A1 PCT/JP2021/031162 JP2021031162W WO2022045196A1 WO 2022045196 A1 WO2022045196 A1 WO 2022045196A1 JP 2021031162 W JP2021031162 W JP 2021031162W WO 2022045196 A1 WO2022045196 A1 WO 2022045196A1
Authority
WO
WIPO (PCT)
Prior art keywords
sputtering target
mass
solder layer
solder
target material
Prior art date
Application number
PCT/JP2021/031162
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English (en)
Japanese (ja)
Inventor
晋 岡野
健志 大友
Original Assignee
三菱マテリアル株式会社
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by 三菱マテリアル株式会社 filed Critical 三菱マテリアル株式会社
Publication of WO2022045196A1 publication Critical patent/WO2022045196A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C13/00—Alloys based on tin
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • 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 sputtering target in which a sputtering target material and a backing material are joined via a solder layer.
  • a sputtering method using a sputtering target is widely used as a means for forming a thin film such as a metal film or an oxide film.
  • the sputtering target has a structure in which a sputtering target material formed according to the composition of the thin film to be formed and a backing material holding the sputtering target material are joined via a solder layer.
  • sputtering target for example, a flat plate type sputtering target having a circular or rectangular target sputtering surface and a cylindrical sputtering target having a cylindrical target sputtering surface are used.
  • the flat plate type sputtering target has a structure in which a flat plate type sputtering target material and a flat plate type backing material (backing plate) are laminated.
  • the cylindrical sputtering target has a structure in which a cylindrical backing material (backing tube) is inserted on the inner peripheral side of the cylindrical sputtering target material.
  • the above-mentioned backing material is arranged for holding the sputtering target material, supplying electric power to the sputtering target material, and cooling the sputtering target material.
  • the backing is performed with the sputtering target material. It needs to be well joined to the material.
  • the In-based solder material is widely used as the solder material constituting the solder layer disposed between the backing material and the sputtering target material.
  • the liquid phase appearance temperature is relatively low, so that the heat resistance is insufficient.
  • the power density at the time of sputter film formation tends to be high, and it is required to improve the heat resistance of the solder layer more than before.
  • Patent Documents 1 and 2 propose Sn—In—Zn-based solders containing Sn, In, and Zn. These Sn—In—Zn-based solders have a higher liquid phase appearance temperature than In-based solders, and can improve the heat resistance of the solder layer formed when soldering.
  • the Zn content in the solder is 8% by mass or more. Since Zn is an element that is easily oxidized, when the sputtering target material and the backing material are bonded using a solder material, the oxidized Zn oxide may be mixed in the solder layer, resulting in poor bonding. .. Further, in Patent Document 2, the content of In in the solder is 30% by mass or more. If the content of In is large, a low melting point compound of In and Sn may be formed, and the heat resistance of the solder layer may be insufficient.
  • the present invention has been made in view of the above-mentioned circumstances, and the sputtering target material and the backing material are surely bonded to each other via a solder layer having excellent heat resistance, and a stable sputtering film formation is performed. It is intended to provide a suitable sputtering target.
  • the sputtering target of the present invention is a sputtering target in which a sputtering target material and a backing material are bonded via a solder layer, and the solder layer contains 9.0 mass% or more of In. Composition containing 15.0 mass% or less, Zn in the range of 4.0 mass% or more and 7.5 mass% or less, Ag in the range of 0 mass% or more and 1.00 mass% or less, and the balance consisting of Sn and unavoidable impurities. It is characterized by being said to be.
  • the sputtering target of the present invention having such a configuration, since the Zn content in the solder layer is 4.0 mass% or more, the melting point of the solder layer is high and the heat resistance is excellent. On the other hand, since the Zn content is 7.5 mass% or less, the mixing of oxidized Zn oxide into the solder layer is suppressed, and the bonding strength between the sputtering target material and the backing material is increased. Further, since the content of In in the solder layer is 9.0 mass% or more, the wettability of the solder material constituting the solder layer is improved, and the sputtering target material and the backing material are well bonded. On the other hand, since the content of In in the solder layer is 15.0 mass% or less, a low melting point compound is not generated and the heat resistance of the solder layer is excellent.
  • the solder layer may further contain Ag in the range of 0.01 mass% or more and 1.00 mass% or less.
  • the solder layer since the solder layer further contains Ag in the range of 0.01 mass% or more and 1.00 mass% or less, the heat resistance of the solder layer can be further improved. Further, Ag can improve the ductility of the solder layer and further improve the strength of the solder layer.
  • the sputtering target material may have a cylindrical shape
  • the backing material may be arranged on the inner peripheral side of the sputtering target material.
  • the sputtering target material since the sputtering target material has a cylindrical shape, the outer peripheral surface of the sputtering target is regarded as the sputtering surface. Therefore, since sputtering is performed while rotating this sputtering target, it is suitable for continuous film formation as compared with the case where a flat plate type sputtering target is used, and the usage efficiency of the sputtering target is excellent. Since the solder layer has the above-mentioned composition, the cylindrical sputtering target material and the backing material can be firmly bonded to each other.
  • the sputtering target material and the backing material are reliably bonded to each other via a solder layer having excellent heat resistance, and the sputtering target capable of stably forming a sputtering film. Can be provided.
  • the sputtering target 10 has a hollow cylindrical sputtering target material 11 extending along the axis O and an inner peripheral side of the sputtering target material 11. It is a cylindrical sputtering target with an inserted hollow cylindrical backing tube 12. The cylindrical sputtering target material 11 and the backing tube 12 are joined to each other via the solder layer 13.
  • the sputtering target material 11 has a composition corresponding to the composition of the thin film to be formed, and is composed of various metals, oxides, and the like.
  • various metals include copper, copper alloys, silver, silver alloys, niobium, niobium alloys, aluminum, aluminum alloys, chromium, chrome alloys, iron alloys, stainless steel and the like.
  • various oxides include AZO, ITO, iron oxide, Cu-CuO and the like.
  • the sputtering target material 11 is composed of an oxide containing zirconium (Zr), silicon (Si) and indium (In).
  • the size of the cylindrical sputtering target material 11 is, for example, an outer diameter DT within the range of 150 mm ⁇ DT ⁇ 170 mm, an inner diameter d T within the range of 120 mm ⁇ d T ⁇ 140 mm, and a length L in the axis O direction.
  • T is within the range of 150 mm ⁇ LT ⁇ 3000 mm.
  • the length LT in the axis O direction may be set to a predetermined size by arranging a plurality of short-sized sputtering target materials 11 adjacent to each other in the axis O direction.
  • the backing tube 12 is provided to hold the cylindrical sputtering target material 11 to secure mechanical strength, and further supplies power to the cylindrical sputtering target material 11 and has a cylindrical shape. It has a function of cooling the sputtering target material 11. Therefore, the backing tube 12 is required to have excellent mechanical strength, electrical conductivity, and thermal conductivity, and is made of, for example, stainless steel such as SUS304, titanium, or the like.
  • the size of the backing tube 12 is, for example, the outer diameter DB is within the range of 119 mm ⁇ DB ⁇ 139 mm, the inner diameter dB is within the range of 110 mm ⁇ dB ⁇ 130 mm, and the length LB in the axis O direction is 200 mm. It is within the range of ⁇ LB ⁇ 3100 mm.
  • the solder layer 13 interposed between the cylindrical sputtering target material 11 and the backing tube 12 is formed when the cylindrical sputtering target material 11 and the backing tube 12 are joined to each other using the solder material. ..
  • the thickness t of the solder layer 13 is within the range of 0.5 mm ⁇ t ⁇ 4 mm.
  • the solder layer 13 contains In in the range of 9.0 mass% or more and 15.0 mass% or less, and Zn in the range of 4.0 mass% or more and 7.5 mass% or less. Ag is contained in the range of 0 mass% or more and 1.00 mass% or less, and the balance is composed of Sn and unavoidable impurities. In the present embodiment, the solder layer 13 may further contain Ag in the range of 0.01 mass% or more and 1.00 mass% or less in addition to Sn, In and Zn.
  • the Zn has the effect of increasing the melting point of the solder layer 13 and improving the heat resistance.
  • the Zn content is less than 4.0 mass%, the above-mentioned effects may not be fully achieved.
  • the Zn content exceeds 7.5 mass%, a large amount of oxide is generated, and the oxidized Zn oxide may be mixed in the solder layer 13 to reduce the bonding strength. Therefore, in the present embodiment, the Zn content in the solder layer 13 is set within the range of 4.0 mass% or more and 7.5 mass% or less.
  • the lower limit of the Zn content in the solder layer 13 is preferably 4.5 mass% or more, and more preferably 5.0 mass% or more.
  • the upper limit of the Zn content in the solder layer 13 is preferably 7.0 mass% or less, preferably 6.5 mass% or less. Is more preferable.
  • the content of In is set within the range of 9.0 mass% or more and 15.0 mass% or less.
  • the lower limit of the content of In in the solder layer 13 is preferably 10.0 mass% or more, and more preferably 11.0 mass% or more.
  • the upper limit of the content of In in the solder layer 13 is preferably 14.0 mass% or less, and more preferably 13.0 mass% or less.
  • the heat resistance of the solder layer 13 can be further improved and the strength can be improved by setting the Ag content in the solder layer 13 to 0.01 mass% or more. Become. On the other hand, by limiting the Ag content in the solder layer 13 to 1.00 mass% or less, it is possible to suppress the deterioration of the wettability of the solder material constituting the solder layer 13 with respect to the sputtering target material 11 and the backing tube 12.
  • the lower limit of the Ag content is preferably 0.02 mass% or more, and more preferably 0.04 mass% or more.
  • the upper limit of the Ag content is preferably 0.75 mass% or less, and more preferably 0.50 mass% or less.
  • a base layer is formed by undercoating the inner peripheral surface of the sputtering target material 11 and the outer peripheral surface of the backing tube 12, which are the joint surfaces, with the base solder.
  • the sputtering target material 11 and the backing tube 12 are heated, and the molten base solder is applied while applying ultrasonic vibration with an ultrasonic iron or the like equipped with a heater to apply the base layer.
  • the heating temperature in the undercoating step S01 is within the range of 160 ° C. or higher and 300 ° C. or lower.
  • the base solder forming the base layer is an In, Sn or Sn—In alloy.
  • the base solder used in the undercoating step S01 contains any of In, Sn and Sn—In alloys.
  • Zn is contained as an impurity, the Zn content is set to less than 0.5 mass%.
  • Zn which is an easily oxidizing element, is intentionally not contained, and impurities are limited to less than 0.5 mass%.
  • the base solder forming the base layer in the undercoat step S01 contains an In, Sn or Sn—In alloy, and when Zn is further contained as an impurity, the Zn content is less than 0.5 mass%.
  • the Zn content is preferably 0.3 mass% or less, and more preferably 0.1 mass% or less.
  • solder joining process S04 Next, the bonding solder is melted and poured into the gap between the inner peripheral surface of the assembled sputtering target material 11 and the outer peripheral surface of the backing tube 12, and then cooled and solidified to form the sputtering target material 11 and the backing tube 12. Solder joint.
  • the heating conditions in the solder joining step S04 are such that the heating temperature is within the range of 160 ° C. or higher and 300 ° C. or lower, and the holding time at this heating temperature is within the range of 30 minutes or longer and 300 minutes or lower.
  • the solder for joining has a composition in which Zn is 4.0 mass% or more and 7.5 mass% or less, In is 9.0 mass% or more and 15.0 mass% or less, and the balance is Sn and unavoidable impurities. Further, Ag may be further contained in the range of 0.01 mass% or more and 1.00 mass% or less.
  • solder joining step S04 Zn contained in the solder for joining is diffused to the base layer side, so that even when a base layer containing no Zn is formed, it is formed after joining.
  • the solder layer 13 is composed of a Sn—In—Zn-based alloy containing Sn, In and Zn.
  • the sputtering target 10 of the present embodiment is manufactured by the process as described above.
  • the melting point of the solder layer 13 becomes high and the heat resistance is high. Excellent in sex.
  • the Zn content is 7.5 mass% or less, the mixing of oxidized Zn oxide into the solder layer 13 is suppressed, and the bonding strength between the sputtering target material 11 and the backing material 12 is increased. ..
  • the In content in the solder layer 13 is 9.0 mass% or more, the wettability of the solder material constituting the solder layer 13 is improved, and the sputtering target material 11 and the backing material 12 are firmly connected. Can be joined.
  • the content of In in the solder layer 13 is 15.0 mass% or less, a low melting point compound is not generated, and the heat resistance of the solder layer 13 is excellent.
  • the solder layer 13 when the solder layer 13 further contains Ag in the range of 0.01 mass% or more and 1.00 mass% or less, the heat resistance of the solder layer 13 can be further improved. Become. Further, the ductility is improved by Ag, and the strength of the solder layer 13 can be further improved.
  • the sputtering target material 11 has a cylindrical shape
  • the backing tube 12 is arranged on the inner peripheral side of the sputtering target material 11, so that the outer peripheral surface of the sputtering target 10 is sputtered.
  • Sputtering is performed while rotating the sputtering target 10 as a surface, which is suitable for continuous film formation as compared with the case where a flat plate type sputtering target is used, and the use efficiency of the sputtering target 10 is excellent. Since the solder layer 13 has the above-mentioned composition, the cylindrical sputtering target material 11 and the backing tube 12 can be firmly bonded to each other.
  • the present invention is not limited to this, and can be appropriately changed without departing from the technical idea of the invention.
  • the cylindrical sputtering targets shown in FIGS. 1A and 1B have been described as examples, but the present invention is not limited to this, and for example, a split type or dogbone type cylindrical sputtering target may be used. There may be. Further, in the present embodiment, the cylindrical sputtering target has been described as an example, but a sputtering target having another shape such as a flat plate shape may be used.
  • a sputtering target material made of the materials shown in Table 1 and a backing tube were prepared.
  • the size of the sputtering target material was 162 mm for the outer diameter DT, 135 mm for the inner diameter d T , and 150 mm for the axial length LT .
  • the size of the backing tube was 133 mm for the outer diameter DB , 125 mm for the inner diameter dB, and 200 mm for the axial length LB.
  • the base solder shown in Tables 1 and 2 and the joining solder shown in Tables 1 and 2 were prepared. Then, the base layer is formed using the base solders shown in Tables 1 and 2, and then cooled to room temperature, the sputtering target material and the backing tube are assembled, and after heating at 200 ° C. for 60 minutes, Tables 1 and 2 are used. Using the soldering material for bonding shown in 2, solder bonding was performed in an atmospheric atmosphere under the condition of holding at 200 ° C. for 1 hour.
  • the sputtering target obtained as described above was evaluated as follows regarding the composition of the solder layer, the bonding ratio, the bonding strength, and the presence or absence of solder melting after sputtering.
  • composition of solder layer The obtained cylindrical sputtering target was cut, and the solder layer was cut out with a cutter knife and 1 g was sampled. The contents of various elements were measured by ICP (inductively coupled plasma).
  • the bonding ratio at the interface between the sputtering target material and the backing tube was evaluated using an ultrasonic flaw detector (SDS-Win 24000T manufactured by Japan Cloud Kramer Co., Ltd.) and calculated from the following formula.
  • the initial joining area is the area to be joined before joining.
  • the peeling is shown by the white part in the joint part, so the area of this white part was defined as the non-joint part area.
  • (Joining ratio) [ ⁇ (Initial joining area)-(Non-joining area) ⁇ / (Initial joining area)] ⁇ 100
  • Comparative Example 1 in which the Zn content in the solder layer was 9.99 mass% and Comparative Example 2 in which the Zn content was 8 mass%, the bonding ratio and the bonding strength were low. Further, since the sputtering target material and the backing tube were not sufficiently bonded, it was confirmed that the solder layer was melted after sputtering. It is presumed that this is because the oxidized Zn oxide is mixed in the solder layer.
  • Comparative Example 3 in which the In content in the solder layer was 17.01 mass% and the Zn content was 0.49 mass%, the melting point of the solder layer was low, and melting of the solder layer was confirmed after sputtering.
  • Comparative Example 4 in which the Ag content in the solder layer was 3.00 mass%, the bonding ratio and the bonding strength were low. Further, since the sputtering target material and the backing tube were not sufficiently bonded, it was confirmed that the solder layer was melted after sputtering. It is presumed that the wettability of the solder material has decreased.
  • Example 1-19 of the present invention in which the Zn content, the In content, and the Ag content in the solder layer are within the range of the present invention, the bonding ratio and the bonding strength are excellent.
  • the soldering target material and the backing material could be joined with sufficient strength. Further, the melting of the solder layer was not confirmed after spattering, and the heat resistance was excellent.
  • the sputtering target material and the backing material are surely bonded to each other via the solder layer having excellent heat resistance, and it is possible to stably perform a sputtering film formation. It was confirmed that a sputtering target can be provided.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

L'invention concerne une cible de pulvérisation qui est construite en joignant ensemble un matériau de cible de pulvérisation et un matériau de support par le biais d'une couche de soudure, et elle est caractérisée en ce que la couche de soudure présente une composition contenant de l'In dans la plage allant de 9,0 % en masse à 15,0 % en masse, du Zn dans la gamme allant de 4,0 % en masse à 7,5 % en masse, et le reste étant du Sn et les impuretés inévitables.
PCT/JP2021/031162 2020-08-26 2021-08-25 Cible de pulvérisation WO2022045196A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2020-142941 2020-08-26
JP2020142941A JP2022038434A (ja) 2020-08-26 2020-08-26 スパッタリングターゲット

Publications (1)

Publication Number Publication Date
WO2022045196A1 true WO2022045196A1 (fr) 2022-03-03

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PCT/JP2021/031162 WO2022045196A1 (fr) 2020-08-26 2021-08-25 Cible de pulvérisation

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JP (1) JP2022038434A (fr)
TW (1) TW202223129A (fr)
WO (1) WO2022045196A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09174278A (ja) * 1995-12-27 1997-07-08 Hitachi Ltd 無鉛はんだ合金およびそれを用いた電子回路装置
CN102409300A (zh) * 2011-09-07 2012-04-11 三峡大学 氧化物陶瓷溅射靶及其制备方法和所用的钎焊合金
US20130029178A1 (en) * 2011-07-27 2013-01-31 Shih-Ying Chang Active solder
WO2014034863A1 (fr) * 2012-08-31 2014-03-06 千住金属工業株式会社 Matériau de liaison électroconducteur

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09174278A (ja) * 1995-12-27 1997-07-08 Hitachi Ltd 無鉛はんだ合金およびそれを用いた電子回路装置
US20130029178A1 (en) * 2011-07-27 2013-01-31 Shih-Ying Chang Active solder
CN102409300A (zh) * 2011-09-07 2012-04-11 三峡大学 氧化物陶瓷溅射靶及其制备方法和所用的钎焊合金
WO2014034863A1 (fr) * 2012-08-31 2014-03-06 千住金属工業株式会社 Matériau de liaison électroconducteur

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JP2022038434A (ja) 2022-03-10
TW202223129A (zh) 2022-06-16

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