JP2014091852A - Gallium nitride target - Google Patents
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Abstract
Description
本発明は、スパッタリング法により窒化ガリウム薄膜を製造する際に使う窒化ガリウムターゲットに関するものである。詳しくは、高温でスパッタを行っても金属部材との接合部分が剥がれない窒化ガリウムターゲットに関するものである。 The present invention relates to a gallium nitride target used when manufacturing a gallium nitride thin film by a sputtering method. Specifically, the present invention relates to a gallium nitride target in which a joint portion with a metal member is not peeled even when sputtering is performed at a high temperature.
窒化ガリウムは、青色発光ダイオード（ＬＥＤ）の発光層や青色レーザーダイオード（ＬＤ）の原料として注目され、近年では薄膜や基板の形態にて白色ＬＥＤや青色ＬＤなどの様々な用途に用いられており、また将来的にはパワーデバイスなどの用途の材料としても注目されている。 Gallium nitride is attracting attention as a light emitting layer for blue light emitting diodes (LEDs) and a raw material for blue laser diodes (LDs). In the future, it is also attracting attention as a material for applications such as power devices.
窒化ガリウム薄膜の作製法としてはスパッタ法が挙げられるが、窒化ガリウムは焼結しにくいので通常の焼成では密度が５０％までしか向上しないため、ターゲットとして使用するには不向きであった。窒化ガリウムの密度を向上させる方法として、窒化ガリウム焼結体に金属ガリウムを含浸させた成形体が提案されているが（例えば、特許文献１参照）、ガリウムは融点が３０℃程度と低いので、基板を加熱してスパッタすると、ターゲット材も加熱され、ターゲット材からガリウムが析出し、金属部材との接合部にあるＩｎハンダと反応して接合力が弱くなり、ターゲット材と金属部材の接合が剥がれてしまうという問題があった。 As a method for producing a gallium nitride thin film, a sputtering method can be mentioned. However, since gallium nitride is difficult to sinter, the density is improved only to 50% by ordinary firing, so that it is not suitable for use as a target. As a method for improving the density of gallium nitride, a molded body in which a gallium nitride sintered body is impregnated with metal gallium has been proposed (see, for example, Patent Document 1), but gallium has a low melting point of about 30 ° C. When the substrate is heated and sputtered, the target material is also heated, gallium is precipitated from the target material, reacts with In solder at the joint with the metal member, and the bonding force becomes weak, and the target material and the metal member are bonded. There was a problem of peeling off.
ターゲット材と金属部材との接合性を改善する方法として、接合層の一部に合成樹脂からなる層を形成させる方法がある（例えば、特許文献２参照）。しかし、熱伝導性を保つためには合成樹脂層は全面積の１０％以下にする必要があり、金属部材との接合部分の大部分は熱伝導性のあるハンダ層であるので、金属ガリウムが混在した窒化ガリウムターゲットを高温でスパッタした場合、金属ガリウムによりハンダ層が侵食され、接合界面が剥がれてしまう。 As a method for improving the bondability between the target material and the metal member, there is a method in which a layer made of a synthetic resin is formed on a part of the bonding layer (see, for example, Patent Document 2). However, in order to maintain thermal conductivity, the synthetic resin layer needs to be 10% or less of the total area, and most of the joint portion with the metal member is a thermally conductive solder layer. When the mixed gallium nitride target is sputtered at a high temperature, the solder layer is eroded by the metal gallium and the bonding interface is peeled off.
また、ターゲット材と金属部材の接合性を改善する例として、ハンダ層に熱伝導性樹脂からなる層を形成させる方法が提案されているが（例えば、特許文献３参照）、熱伝導性樹脂としてはＡｇフィラーとエポキシ樹脂からなる樹脂しか具体的に開示されておらず、Ａｇはガリウムと反応してしまうため、窒化ガリウムターゲットには適さない。 As an example of improving the bondability between the target material and the metal member, a method of forming a layer made of a heat conductive resin on the solder layer has been proposed (see, for example, Patent Document 3). Only a resin composed of an Ag filler and an epoxy resin is specifically disclosed, and Ag reacts with gallium, so that it is not suitable for a gallium nitride target.
本発明の目的は、窒化ガリウム成形物と金属部材とを接合層を介して接合した窒化ガリウムターゲットにおいて、前記接合層にガリウムと反応しない金属及び導電性の樹脂からなる層を形成することで、高温でスパッタを行っても接合部分が剥がれない窒化ガリウムターゲットを提供することである。 An object of the present invention is to form a layer made of a metal that does not react with gallium and a conductive resin in a gallium nitride target in which a gallium nitride molded product and a metal member are bonded via a bonding layer. The object is to provide a gallium nitride target in which the bonded portion does not peel off even when sputtering is performed at a high temperature.
窒化ガリウムターゲットにおいて、ターゲット材と金属部材とを融点の低いＩｎ系ハンダを接合層としてロウ付けする方法が一般的であるが、ガリウムは融点が約３０℃のため、基板を加熱して窒化ガリウムターゲットをスパッタすると、ターゲット表面にガリウムが析出する場合がある。ガリウムは多くの金属を侵食する性質があるので、ガリウムがＩｎ系ハンダと反応して接合部の接着性が低下し、ターゲット材と金属部材の接合が剥がれてしまうことがある。 In a gallium nitride target, a method in which a target material and a metal member are brazed with In solder having a low melting point as a bonding layer is generally used. However, since gallium has a melting point of about 30 ° C., the substrate is heated to gallium nitride. When the target is sputtered, gallium may be deposited on the target surface. Since gallium has the property of eroding many metals, gallium reacts with In-based solder and adhesion of the joint portion is lowered, and the bond between the target material and the metal member may be peeled off.
そこで本発明者らは、ターゲット材である窒化ガリウム成形物と金属部材とをガリウムと反応しない金属を含む導電性樹脂を介して接合することにより、高温でスパッタを行っても、ターゲット材と金属部材が剥がれないことを見出した。 Therefore, the present inventors joined the target gallium nitride molded product and the metal member through a conductive resin containing a metal that does not react with gallium, so that the target material and the metal can be sputtered at high temperatures. The member was found not to peel off.
すなわち、本発明は、ターゲット材である窒化ガリウム成形物と金属部材とを接合層を介して接合した窒化ガリウムターゲットであって、前記接合層がガリウムと反応しない金属を２０〜６０ｖｏｌ％含む導電性樹脂であることを特徴とする窒化ガリウムターゲットである。 That is, the present invention is a gallium nitride target obtained by bonding a gallium nitride molded product as a target material and a metal member via a bonding layer, and the bonding layer includes 20 to 60 vol% of a metal that does not react with gallium. The gallium nitride target is a resin.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
本発明の窒化ガリウムターゲットは、ターゲット材である窒化ガリウム成形物と金属部材とを接合層を介して接合した窒化ガリウムターゲットである。成形物とは、成形、焼成など様々な方法で粉末を固めたものを含む成形物を指す。本発明において、窒化ガリウム成形物とは窒化ガリウムを主成分とする焼結体、窒化ガリウム焼結体に金属ガリウムを含浸させた成形体などが挙げられる。窒化ガリウム焼結体に金属ガリウムを含浸させた成形体では、金属ガリウムが窒化ガリウム焼結体の空隙に存在しているため、スパッタ中にターゲット材からガリウムが析出するという事態が起こりやすく、特に本発明が好適に利用されうる。 The gallium nitride target of the present invention is a gallium nitride target in which a gallium nitride molded product as a target material and a metal member are bonded via a bonding layer. The molded product refers to a molded product including those obtained by solidifying powder by various methods such as molding and baking. In the present invention, the gallium nitride molded product includes a sintered body containing gallium nitride as a main component, a molded body obtained by impregnating a gallium nitride sintered body with metal gallium, and the like. In a molded body in which metal gallium is impregnated into a gallium nitride sintered body, since the metal gallium is present in the voids of the gallium nitride sintered body, a situation in which gallium is likely to precipitate from the target material during sputtering is particularly likely. The present invention can be suitably used.
本発明において、接合層に用いられるガリウムと反応しない金属を含む導電性樹脂とは、タングステン、タンタルをフィラーとするエポキシ樹脂、ウレタン樹脂、ポリエステル樹脂などが挙げられる。熱伝導率が高いことからタングステンをフィラーとする樹脂を用いることが好ましい。 In the present invention, examples of the conductive resin containing a metal that does not react with gallium used for the bonding layer include tungsten, an epoxy resin containing tantalum as a filler, a urethane resin, and a polyester resin. It is preferable to use a resin containing tungsten as a filler because of its high thermal conductivity.
また、ガリウムと反応しない金属は樹脂に対して、２０〜６０ｖｏｌ％含まれていることを特徴とし、３０〜５０ｖｏｌ％含まれていることが好ましい。２０ｖｏｌ％未満であると、熱伝導率が不十分となることがあり、６０ｖｏｌ％を超えると接着性が低下し、加熱した際に接合が剥がれてしまう場合がある。 Further, the metal that does not react with gallium is contained in an amount of 20 to 60% by volume, and preferably 30 to 50% by volume, based on the resin. If it is less than 20 vol%, the thermal conductivity may be insufficient, and if it exceeds 60 vol%, the adhesiveness may be lowered and the bond may be peeled off when heated.
導電性樹脂の熱伝導率は１Ｗ／ｍＫ以上であることが好ましい。熱伝導率が１Ｗ／ｍＫ未満であると、熱伝導が不十分となってターゲット材の温度が急激に上昇してしまい、破損するおそれがある。熱伝導率は、例えばＪＩＳ Ｒ １６１１に記載されているレーザーフラッシュ法により測定できる。 The heat conductivity of the conductive resin is preferably 1 W / mK or more. If the thermal conductivity is less than 1 W / mK, the thermal conductivity becomes insufficient and the temperature of the target material rises rapidly, which may cause damage. The thermal conductivity can be measured by, for example, a laser flash method described in JIS R 1611.
本発明によれば、窒化ガリウム成形物と金属部材とをガリウムと反応しない金属を含む導電性樹脂を介して接合することにより、高温で成膜を行っても窒化ガリウム成形物と接合部が剥がれない窒化ガリウムターゲットを製造することが可能である。 According to the present invention, by bonding a gallium nitride molded product and a metal member via a conductive resin containing a metal that does not react with gallium, the gallium nitride molded product and the joint are peeled even when film formation is performed at a high temperature. It is possible to produce a non-gallium nitride target.
以下、本発明の実施例をもって説明するが、本発明はこれに限定されるものではない。なお、窒化ガリウムと金属ガリウムが混在した成形物の詳細な製造方法については特許文献１を参照のこと。 Examples of the present invention will be described below, but the present invention is not limited thereto. Refer to Patent Document 1 for a detailed manufacturing method of a molded product in which gallium nitride and metal gallium are mixed.
（実施例１）
窒化ガリウムと金属ガリウムが混在した成形物（サイズ７６．２ｍｍφ×３．５ｍｍｔ、密度５．２ｇ／ｃｍ３）に、６０ｖｏｌ％のエポキシ樹脂と４０ｖｏｌ％のタングステンフィラーをよく混合した導電性樹脂（熱伝導率２Ｗ／ｍＫ）を全面に塗布し、Ｃｕ製バッキングプレートと接合した。
Example 1
Conductive resin (heat) in which 60 vol% epoxy resin and 40 vol% tungsten filler are well mixed with a molded product (size 76.2 mmφ × 3.5 mmt, density 5.2 g / cm 3 ) mixed with gallium nitride and metal gallium. A conductivity of 2 W / mK) was applied to the entire surface and joined to a Cu backing plate.
作製した窒化ガリウムターゲットを２００℃で２時間加熱し、加熱後の成形物と金属部材との接合性を調べたところ、強固に結びついており剥がれなかった。 When the produced gallium nitride target was heated at 200 ° C. for 2 hours and the bonding property between the heated molded product and the metal member was examined, the gallium nitride target was firmly bonded and did not peel off.
（実施例２）
窒化ガリウムと金属ガリウムが混在した成形物（サイズ７６．２ｍｍφ×３．５ｍｍｔ、密度５．２ｇ／ｃｍ３）に、６０ｖｏｌ％のウレタン樹脂と４０ｖｏｌ％のタングステンフィラーをよく混合した導電性樹脂（熱伝導率２Ｗ／ｍＫ）を全面に塗布し、Ｃｕ製バッキングプレートと接合した。
(Example 2)
Conductive resin (heat) in which 60 vol% urethane resin and 40 vol% tungsten filler are well mixed with a molded product (size 76.2 mmφ × 3.5 mmt, density 5.2 g / cm 3 ) mixed with gallium nitride and metal gallium. A conductivity of 2 W / mK) was applied to the entire surface and joined to a Cu backing plate.
作製した窒化ガリウムターゲットを２００℃で２時間加熱し、加熱後の成形物と金属部材との接合性を調べたところ、強固に結びついており剥がれなかった。 When the produced gallium nitride target was heated at 200 ° C. for 2 hours and the bonding property between the heated molded product and the metal member was examined, the gallium nitride target was firmly bonded and did not peel off.
（実施例３）
窒化ガリウムと金属ガリウムが混在した成形物（サイズ７６．２ｍｍφ×３．５ｍｍｔ、密度５．２ｇ／ｃｍ３）に、７０ｖｏｌ％のエポキシ樹脂と３０ｖｏｌ％のタングステンフィラーをよく混合した導電性樹脂（熱伝導率１．５Ｗ／ｍＫ）を全面に塗布し、Ｃｕ製バッキングプレートと接合した。
(Example 3)
Conductive resin (heat) in which a mixture of gallium nitride and metal gallium (size 76.2 mmφ × 3.5 mmt, density 5.2 g / cm 3 ) is well mixed with 70 vol% epoxy resin and 30 vol% tungsten filler. A conductivity of 1.5 W / mK) was applied to the entire surface and joined to a Cu backing plate.
作製した窒化ガリウムターゲットを２００℃で２時間加熱し、加熱後の成形物と金属部材との接合性を調べたところ、強固に結びついており剥がれなかった。
（実施例４）
窒化ガリウムと金属ガリウムが混在した成形物（サイズ７６．２ｍｍφ×３．５ｍｍｔ、密度５．２ｇ／ｃｍ３）に、４５ｖｏｌ％のエポキシ樹脂と５５ｖｏｌ％のタングステンフィラーをよく混合した導電性樹脂（熱伝導率４．５Ｗ／ｍＫ）を全面に塗布し、Ｃｕ製バッキングプレートと接合した。
When the produced gallium nitride target was heated at 200 ° C. for 2 hours and the bonding property between the heated molded product and the metal member was examined, the gallium nitride target was firmly bonded and did not peel off.
(Example 4)
Conductive resin (heat) in which 45 vol% epoxy resin and 55 vol% tungsten filler are well mixed in a molded product containing gallium nitride and metal gallium (size 76.2 mmφ × 3.5 mmt, density 5.2 g / cm 3 ). Conductivity 4.5 W / mK) was applied to the entire surface and joined to a Cu backing plate.
作製した窒化ガリウムターゲットを２００℃で２時間加熱し、加熱後の成形物と金属部材との接合性を調べたところ、強固に結びついており剥がれなかった。 When the produced gallium nitride target was heated at 200 ° C. for 2 hours and the bonding property between the heated molded product and the metal member was examined, the gallium nitride target was firmly bonded and did not peel off.
（比較例１）
窒化ガリウムと金属ガリウムが混在した成形物（サイズ７６．２ｍｍφ×３．５ｍｍｔ、密度５．２ｇ／ｃｍ３）に１０００ｎｍのＣｕ薄膜を形成し、Ｉｎハンダ（熱伝導率８１．６Ｗ／ｍＫ）を全面に塗布し、Ｃｕ製バッキングプレートと接合した。
(Comparative Example 1)
A 1000 nm Cu thin film is formed on a molded product (size 76.2 mmφ × 3.5 mmt, density 5.2 g / cm 3 ) containing gallium nitride and metal gallium, and In solder (thermal conductivity 81.6 W / mK) is used. It was applied to the entire surface and joined to a Cu backing plate.
作製した窒化ガリウムターゲットを２００℃で２時間加熱し、加熱後の成形物と金属部材の接合性を調べたところ、加熱後は基板と成型物は容易に動き、剥がれた。 The produced gallium nitride target was heated at 200 ° C. for 2 hours, and the bondability between the heated molded product and the metal member was examined. After the heating, the substrate and the molded product easily moved and peeled off.
（比較例２）
窒化ガリウムと金属ガリウムが混在した成形物（サイズ７６．２ｍｍφ×３．５ｍｍｔ、密度５．２ｇ／ｃｍ３）に、７０ｖｏｌ％のエポキシ樹脂と３０ｖｏｌ％のＡｇフィラーをよく混合した導電性樹脂（熱伝導率４Ｗ／ｍＫ）を全面に塗布し、Ｃｕ製バッキングプレートと接合した。
(Comparative Example 2)
Conductive resin (heat) in which a mixture of gallium nitride and metal gallium (size 76.2 mmφ × 3.5 mmt, density 5.2 g / cm 3 ) is well mixed with 70 vol% epoxy resin and 30 vol% Ag filler. Conductivity 4 W / mK) was applied to the entire surface and joined to a Cu backing plate.
作製した窒化ガリウムターゲットを２００℃で２時間加熱し、加熱後の成形物と金属部材との接合性を調べたところ、加熱後は基板と成型物は容易に動き、剥がれた。 The produced gallium nitride target was heated at 200 ° C. for 2 hours, and the bondability between the heated molded product and the metal member was examined. After the heating, the substrate and the molded product easily moved and peeled off.
（比較例３）
窒化ガリウムと金属ガリウムが混在した成形物（サイズ７６．２ｍｍφ×３．５ｍｍｔ、密度５．２ｇ／ｃｍ３）に、３０ｖｏｌ％のエポキシ樹脂と７０ｖｏｌ％のタングステンフィラーをよく混合した導電性樹脂（熱伝導率９Ｗ／ｍＫ）を全面に塗布し、Ｃｕ製バッキングプレートと接合した。
(Comparative Example 3)
Conductive resin (heat) in which 30 vol% epoxy resin and 70 vol% tungsten filler are well mixed with a molded product (size 76.2 mmφ × 3.5 mmt, density 5.2 g / cm 3 ) mixed with gallium nitride and metal gallium. A conductivity of 9 W / mK) was applied to the entire surface and joined to a Cu backing plate.
作製した窒化ガリウムターゲットを２００℃で２時間加熱し、加熱後の成形物と金属部材との接合性を調べたところ、接合層が剥離し、基板と成型物は剥がれた。 When the produced gallium nitride target was heated at 200 ° C. for 2 hours and the bonding property between the heated molded product and the metal member was examined, the bonding layer was peeled off, and the substrate and the molded product were peeled off.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016009577A1 (en) * | 2014-07-18 | 2016-01-21 | キヤノンアネルバ株式会社 | Method for forming nitride semiconductor layer and method for manufacturing semiconductor device |
| JP2021181595A (en) * | 2020-05-18 | 2021-11-25 | 東京エレクトロン株式会社 | Composite target, manufacturing method of composite target, formation method of nitride semiconductor film |
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| JP6001194B2 (en) * | 2014-07-18 | 2016-10-05 | キヤノンアネルバ株式会社 | Method for forming nitride semiconductor layer and method for manufacturing semiconductor device |
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