JP5656135B2 - Cu-based wiring film - Google Patents

Cu-based wiring film Download PDF

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JP5656135B2
JP5656135B2 JP2013185185A JP2013185185A JP5656135B2 JP 5656135 B2 JP5656135 B2 JP 5656135B2 JP 2013185185 A JP2013185185 A JP 2013185185A JP 2013185185 A JP2013185185 A JP 2013185185A JP 5656135 B2 JP5656135 B2 JP 5656135B2
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村田　英夫
英夫 村田
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Hitachi Metals Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/52—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames
    • H01L23/522—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body
    • H01L23/532—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames including external interconnections consisting of a multilayer structure of conductive and insulating layers inseparably formed on the semiconductor body characterised by the materials
    • H01L23/53204—Conductive materials
    • H01L23/53209—Conductive materials based on metals, e.g. alloys, metal silicides
    • H01L23/53228—Conductive materials based on metals, e.g. alloys, metal silicides the principal metal being copper
    • H01L23/53238—Additional layers associated with copper layers, e.g. adhesion, barrier, cladding layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
    • H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
    • H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/52—Arrangements for conducting electric current within the device in operation from one component to another, i.e. interconnections, e.g. wires, lead frames
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Computer Hardware Design (AREA)
  • Physics & Mathematics (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)
  • Liquid Crystal (AREA)
  • Physical Vapour Deposition (AREA)
  • Devices For Indicating Variable Information By Combining Individual Elements (AREA)
  • Electrodes Of Semiconductors (AREA)
  • Parts Printed On Printed Circuit Boards (AREA)
  • Manufacturing Of Printed Wiring (AREA)

Description

本発明は、平面表示装置に用いられるＣｕ系配線膜に関するものである。   The present invention relates to a Cu-based wiring film used in a flat display device.

薄膜デバイスを作製する液晶ディスプレイ、プラズマディスプレイパネル、有機エレクトロルミネッセンスディスプレイ等の平面表示装置に用いられる配線膜には、従来から耐食性、耐熱性、基板との密着性に優れる金属であるＭｏやＭｏを主成分とする合金が用いられている（例えば、特許文献１参照）。しかしながら、近年、Ｍｏは原料価格が高騰しており、より価格の安い代替の金属材料としてＣｕ等が検討されている。   For wiring films used in flat display devices such as liquid crystal displays, plasma display panels, and organic electroluminescence displays that produce thin film devices, Mo and Mo, which are metals with excellent corrosion resistance, heat resistance, and adhesion to substrates, have been used. An alloy having a main component is used (for example, see Patent Document 1). However, in recent years, the raw material price of Mo has soared, and Cu or the like has been studied as an alternative metal material with a lower price.

特開２００２−１９０２１２号公報JP 2002-190212 A

Ｃｕは、Ｍｏに比べて低価格な金属材料であるが、Ｃｕを配線膜に適用する場合には、基板に対する密着性が弱いという問題がある。
本発明の目的は、上記の課題に鑑み、基板との密着性を向上することが可能な新規なＣｕ系配線膜を提供することである。 Cu is a metal material that is less expensive than Mo. However, when Cu is applied to a wiring film, there is a problem that adhesion to a substrate is weak.
In view of the above problems, an object of the present invention is to provide a novel Cu-based wiring film capable of improving adhesion to a substrate.

本発明者は、Ｃｕ系配線膜として、Ｃｕ２Ｏを一定量含んだＣｕからなる膜に制御することで、基板との密着性を向上させるが可能となることを見出し本発明に到達した。
すなわち、本発明は、ガラス基板上に形成されるＣｕ酸化物を有するＣｕ系配線膜であって、Ｃｕの主結晶面（１１１）面のＸ線回折ピーク強度をＣｕ（１１１）、Ｃｕ２Ｏの主結晶面（１１１）面のＸ線回折のピーク強度をＣｕ２Ｏ（１１１）とした場合に、その強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）の値が０．８〜２．５の範囲にあるＣｕ系配線膜である。
また、好ましくは、膜厚が２００〜５００ｎｍである前記Ｃｕ系配線膜である。
また、好ましくは、比抵抗が１５μΩｃｍ以下の前記Ｃｕ系配線膜である。
また、前記Ｃｕ系配線膜上にＣｕ膜が積層される構成も望ましい。 The present inventor has found that the adhesion to the substrate can be improved by controlling the Cu-based wiring film to a film made of Cu containing a certain amount of Cu 2 O, and has reached the present invention.
That is, the present invention is a Cu-based wiring film having Cu oxide formed on a glass substrate, wherein the X-ray diffraction peak intensity of the main crystal plane (111) of Cu is Cu (111), Cu 2 O. of when the peak intensity of X-ray diffraction of the major crystal faces (111) plane was Cu 2 O (111), the value of the intensity ratio Cu (111) / Cu 2 O (111) 0.8~2. Cu-based wiring film in the range of 5.
Moreover, the Cu-based wiring film having a thickness of 200 to 500 nm is preferable.
The Cu-based wiring film having a specific resistance of 15 μΩcm or less is preferable.
A configuration in which a Cu film is laminated on the Cu-based wiring film is also desirable.

本発明によれば、配線材料として価格の安いＣｕ系配線膜として、基板との密着性を向上させることが可能となるので、平面表示装置用の配線膜として欠くことのできない技術となる。   According to the present invention, it is possible to improve the adhesiveness with a substrate as a Cu-based wiring film, which is inexpensive as a wiring material, and this is an indispensable technique as a wiring film for a flat display device.

試料１のＸ線回折パターンである。2 is an X-ray diffraction pattern of Sample 1. 試料５のＸ線回折パターンである。3 is an X-ray diffraction pattern of Sample 5. 試料６のＸ線回折パターンである。2 is an X-ray diffraction pattern of Sample 6.

本発明の最大の特徴は、Ｃｕ系配線膜として、Ｃｕ２Ｏを一定量含んだＣｕからなる膜に制御することで、基板に対する密着性を向上させることが可能となる点にある。
Ｃｕ系配線膜中のＣｕ２Ｏ量に関しては、同定が困難であるため、Ｘ線回折強度測定において、Ｃｕの主結晶面（１１１）面のピーク強度とＣｕ２Ｏの主結晶面（１１１）面のピーク強度の比で特定している。ピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）は０．８〜２．５の範囲とすることで、密着性の向上の効果が十分現れる。好ましくは、ピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）が１．０〜２．０の範囲である。 The greatest feature of the present invention is that the adhesion to the substrate can be improved by controlling the Cu-based wiring film to a film made of Cu containing a certain amount of Cu 2 O.
Since it is difficult to identify the amount of Cu 2 O in the Cu-based wiring film, the peak intensity of the Cu main crystal plane (111) plane and the Cu 2 O main crystal plane (111) are measured in the X-ray diffraction intensity measurement. It is specified by the ratio of the peak intensity of the surface. By making the peak intensity ratio Cu (111) / Cu 2 O (111) in the range of 0.8 to 2.5, the effect of improving the adhesion sufficiently appears. Preferably, the peak intensity ratio Cu (111) / Cu 2 O (111) is in the range of 1.0 to 2.0.

なお、ピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）が０．８に満たない場合には、Ｃｕ系配線膜中のＣｕ２Ｏの含有量が多くなると考えられるため、密着性の向上効果は高いが、比抵抗が上昇し過ぎるため好ましくない。また、ピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）が２．５を超える場合には、Ｃｕ系配線膜中のＣｕ２Ｏの含有量が少ないと考えられるため、密着性の向上が十分ではない。 Since the peak intensity ratio Cu (111) / Cu 2 O (111) is in the case of less than 0.8 is considered to have the content of Cu 2 O in the Cu-based wiring film increases, improvement in adhesion Although the effect is high, it is not preferable because the specific resistance increases excessively. Further, when the peak intensity ratio Cu (111) / Cu 2 O (111) exceeds 2.5, it is considered that the content of Cu 2 O in the Cu-based wiring film is small, so that the adhesion is improved. Not enough.

また、本発明のＣｕ系配線膜は、膜厚が２００〜５００ｎｍであることが好ましい。それは、膜厚が２００ｎｍに満たない場合には、膜が薄いために膜表面の電子散乱の影響によって電気抵抗が上昇してしまうとともに、膜の表面形態が変化しやすく望ましくないためである。また、膜厚が５００ｎｍを超えると、電気抵抗は低く抑えられるが、膜応力によって膜が剥がれ易くなり、成膜に時間がかかり生産効率上望ましくないためである。   The Cu-based wiring film of the present invention preferably has a film thickness of 200 to 500 nm. This is because when the film thickness is less than 200 nm, since the film is thin, the electrical resistance increases due to the influence of electron scattering on the film surface, and the surface form of the film easily changes, which is not desirable. On the other hand, if the film thickness exceeds 500 nm, the electrical resistance can be kept low, but the film is easily peeled off by the film stress, and it takes a long time to form the film, which is undesirable in terms of production efficiency.

また、本発明のＣｕ系配線膜は、比抵抗が１５μΩｃｍ以下であることが好ましい。それは、純Ｍｏ配線膜の比抵抗が１５μΩｃｍ程度であり、Ｍｏ系配線膜の代替材料としては、同一の比抵抗程度以下を実現することが望ましいためである。
なお、本発明のＣｕ系配線膜においては、成膜時に比抵抗が高いものに関しても、成膜後に真空雰囲気中で加熱処理を行うことで、比抵抗を１５μΩｃｍ以下へ低減することが可能である。 In addition, the Cu-based wiring film of the present invention preferably has a specific resistance of 15 μΩcm or less. This is because the specific resistance of the pure Mo wiring film is about 15 μΩcm, and it is desirable to realize the same specific resistance or less as an alternative material for the Mo-based wiring film.
In the Cu-based wiring film of the present invention, even when the specific resistance is high during film formation, the specific resistance can be reduced to 15 μΩcm or less by performing heat treatment in a vacuum atmosphere after film formation. .

また、平面表示装置の配線膜として使用される場合には、駆動素子である薄膜トランジスタ（ＴＦＴ）に用いられるシリコン薄膜上に接して配線膜を形成する場合がある。Ｃｕを配線膜に適用する場合には、このシリコン薄膜との相互拡散反応により駆動素子の特性が劣化するという問題があるが、本発明のピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）が０．８〜２．５の範囲にあるＣｕ系配線膜とすることで相互拡散反応も抑制することも可能となる。 When used as a wiring film of a flat display device, the wiring film may be formed in contact with a silicon thin film used for a thin film transistor (TFT) as a driving element. When Cu is applied to the wiring film, there is a problem that the characteristics of the driving element deteriorate due to the mutual diffusion reaction with the silicon thin film. However, the peak intensity ratio Cu (111) / Cu 2 O (111) By using a Cu-based wiring film in the range of 0.8 to 2.5, it is possible to suppress the mutual diffusion reaction.

また、本発明のピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）が０．８〜２．５の範囲にあるＣｕ系配線膜は、基板に対する密着性を向上させることが可能であるため、さらに、このＣｕ系配線膜上にＣｕ膜を積層させた配線膜を形成することも可能である。この構成を有する配線膜とすることで、基板に対する十分な密着性と積層したＣｕ膜の低抵抗の特性を併せもつことが可能となるためである。 Further, the Cu-based wiring film having the peak intensity ratio Cu (111) / Cu 2 O (111) in the range of 0.8 to 2.5 of the present invention can improve the adhesion to the substrate. Furthermore, it is possible to form a wiring film in which a Cu film is laminated on the Cu-based wiring film. This is because by using the wiring film having this configuration, it is possible to have both sufficient adhesion to the substrate and the low resistance characteristics of the laminated Cu film.

本発明のＣｕ系配線膜を成膜するためには、スパッタリングガスとしてＡｒとＯ２の混合ガスを使用した反応性スパッタにより成膜を行うことが望ましい。また、反応性スパッタにおいてはＯ２分圧、投入電力を制御して、基板との密着性を向上させるために必要なＣｕ２ＯをＣｕ系配線膜中に含有させることが重要となる。 In order to form the Cu-based wiring film of the present invention, it is desirable that the film be formed by reactive sputtering using a mixed gas of Ar and O 2 as a sputtering gas. In reactive sputtering, it is important to contain Cu 2 O necessary for improving the adhesion with the substrate by controlling the O 2 partial pressure and input power in the Cu-based wiring film.

反応性スパッタリングにおけるＯ２分圧は、５％以下では密着性が十分でなく、３０％を超えると低抵抗が大きく増加してしまう。このため、５〜３０％程度に制御することが望ましい。また、スパッタリングにおける投入電力は、成膜速度とＣｕ系配線膜中のＣｕ２Ｏの含有量、さらにタ−ゲット表面での酸化物の生成に影響を与える。スパッタリングの際の投入電力が低いと生産性が低下するとともにＣｕタ−ゲットの表面に酸化物が生成し、パ−ティクル等の異物が発生しやすくなる。また、投入電力を上げすぎると異常放電等が起きやすくなる。よって、スパッタリングの際にパーティクルや異常放電の発生を抑制し、Ｃｕ２Ｏの含有量を適切に制御したＣｕ系配線膜を成膜するため、投入電力はターゲットの表面積あたりの換算で、２〜１０Ｗ／ｃｍ２程度に制御することが望ましい。 If the O 2 partial pressure in the reactive sputtering is 5% or less, the adhesion is not sufficient, and if it exceeds 30%, the low resistance greatly increases. For this reason, it is desirable to control to about 5 to 30%. In addition, the input power in sputtering affects the film formation rate, the Cu 2 O content in the Cu-based wiring film, and the generation of oxide on the target surface. If the input power at the time of sputtering is low, productivity is lowered and oxides are generated on the surface of the Cu target, and foreign matters such as particles are likely to be generated. Further, if the input power is increased too much, abnormal discharge or the like is likely to occur. Therefore, in order to suppress the generation of particles and abnormal discharge during sputtering and to form a Cu-based wiring film in which the content of Cu 2 O is appropriately controlled, the input power is 2 to 2 in terms of the surface area of the target. It is desirable to control to about 10 W / cm 2 .

なお、上記の反応性スパッタリングによって成膜されたＣｕ系配線膜は、真空雰囲気中で加熱することで、比抵抗を低減することが可能となる。その際に、真空雰囲気とするのは、Ｃｕ系配線膜の酸化の進行を防止するためであり、望ましくは、１×１０４Ｐａ以下へ減圧した雰囲気である。また、加熱温度は、Ｃｕ系配線膜中の欠陥の低減とＣｕ２Ｏを安定化させるという理由から、２５０〜４００℃の範囲で加熱することが望ましい。 In addition, it becomes possible to reduce a specific resistance by heating the Cu-type wiring film formed by the above reactive sputtering in a vacuum atmosphere. In this case, the vacuum atmosphere is used to prevent the progress of oxidation of the Cu-based wiring film, and is preferably an atmosphere reduced to 1 × 10 4 Pa or less. The heating temperature is preferably in the range of 250 to 400 ° C. for the reason of reducing defects in the Cu-based wiring film and stabilizing Cu 2 O.

また、本発明のＣｕ系配線膜は、ガラス基板、Ｓｉウェハ基板、樹脂基板等の上に形成することが可能であるが、特に、一般的に平面表示装置を製造するのに使用さているガラス基板上へ形成するのに有効である。   In addition, the Cu-based wiring film of the present invention can be formed on a glass substrate, a Si wafer substrate, a resin substrate, etc., and in particular, glass generally used for manufacturing a flat display device. It is effective for forming on a substrate.

２５×５０ｍｍのガラス基板上（コーニング１７３７）に、純度９９．９９％のＣｕターゲット（直径１６４ｍｍ×厚さ５ｍｍ）、Ｏ２ガスを含んだＡｒガスを用いた反応性スパッタリングによって、膜厚２００ｎｍのＣｕ系配線膜を成膜した。なお、反応性スパッタリングとしては、アネルバ製Ｃ−３０１０のスパッタリング装置、スパッタリング雰囲気中のガス圧０．５Ｐａ、投入電力１０００Ｗの条件で、スパッタリングガス中のＯ２分圧を０〜４０％の範囲で条件を振って、表１に示す試料１〜６のＣｕ系配線膜を作製した。 On a 25 × 50 mm glass substrate (Corning 1737), a reactive sputtering using a 99.99% pure Cu target (diameter 164 mm × thickness 5 mm) and Ar gas containing O 2 gas has a thickness of 200 nm. A Cu-based wiring film was formed. In addition, as reactive sputtering, an O 2 partial pressure in the sputtering gas is within a range of 0 to 40% under the conditions of an Anelva C-3010 sputtering apparatus, a gas pressure in the sputtering atmosphere of 0.5 Pa, and an input power of 1000 W. Under conditions, Cu-based wiring films of Samples 1 to 6 shown in Table 1 were produced.

各試料は、比抵抗を測定するとともに、リガク製Ｘ線回折装置ＲＩＮＴ２５００を使用してＸ線回折強度測定を行いＣｕとＣｕ２Ｏのピーク強度比を評価した。また、密着性試験として、各試料のスパッタリング成膜したＣｕ系配線膜に２ｍｍ間隔で碁盤の目状に切れ目を入れた後、膜表面にテープを貼り、引き剥がした時に基板上に残った桝目を面積率で評価する試験を行った。以上の結果を表１に示す。
また、試料１、５および６のＸ回折強度測定をした際のＸ線回折パターンをそれぞれ図１〜３に示す。
また、各試料を１００Ｐａ以下に減圧した真空雰囲気で温度２５０℃、１時間の加熱処理を行った後に、比抵抗を測定した。その結果も表１に示す。 Each sample measured the specific resistance and measured the X-ray diffraction intensity using a Rigaku X-ray diffractometer RINT2500 to evaluate the peak intensity ratio of Cu and Cu 2 O. In addition, as an adhesion test, the Cu-based wiring film formed by sputtering for each sample was cut into a grid pattern at intervals of 2 mm, and then tape was applied to the film surface, and the grid remaining on the substrate when peeled off. The test which evaluates by area ratio was done. The results are shown in Table 1.
Moreover, the X-ray diffraction pattern at the time of measuring the X diffraction intensity of the samples 1, 5 and 6 is shown in FIGS.
The specific resistance was measured after performing heat treatment at 250 ° C. for 1 hour in a vacuum atmosphere in which each sample was decompressed to 100 Pa or less. The results are also shown in Table 1.

表１から、ピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）が０．８〜２．５の範囲にある試料４および５は、密着性試験において膜剥れが生じておらず十分な密着性を有していることが分かる。
また、試料４および５は、真空雰囲気中で加熱処理を行うことで、比抵抗を１５μΩｃｍ以下へ低減することが可能であることも分かる。 From Table 1, samples 4 and 5 in which the peak intensity ratio Cu (111) / Cu 2 O (111) is in the range of 0.8 to 2.5 are sufficiently free from film peeling in the adhesion test. It turns out that it has adhesiveness.
It can also be seen that samples 4 and 5 can be reduced in specific resistance to 15 μΩcm or less by heat treatment in a vacuum atmosphere.

２５×５０ｍｍのガラス基板上（コーニング１７３７）に、膜厚５０ｎｍのシリコン薄膜を形成した後に、純度９９．９９％のＣｕターゲット（直径１６４ｍｍ×厚さ５ｍｍ）、Ｏ２ガスを含んだＡｒガスを用いた反応性スパッタリングによって、膜厚２００ｎｍのＣｕ系配線膜を成膜した。なお、反応性スパッタリングとしては、アネルバ製Ｃ−３０１０のスパッタリング装置、スパッタリング雰囲気中のガス圧０．５Ｐａ、投入電力１０００Ｗの条件とした。また、スパッタリングガス中のＯ２分圧に関しては、試料１１を０％、試料１２を１４％の条件で成膜をした。
各試料は、比抵抗を測定するとともに、実施例１と同様に、Ｘ線回折強度測定を行いＣｕとＣｕ２Ｏのピーク強度比を評価した。また、ガラス基板側からコニカミノルタ製のＣＭ２００２分光測色計でＳｉ膜の反射率を測定した。
その後、各試料を１００Ｐａ以下に減圧した真空雰囲気で温度２５０℃、１時間の加熱処理を行った。加熱処理後の試料に関しても上記と同様に比抵抗、Ｘ線回折強度、反射率を測定した。以上の結果を表２に示す。 After forming a 50 nm-thick silicon thin film on a 25 × 50 mm glass substrate (Corning 1737), a 99.99% pure Cu target (diameter 164 mm × thickness 5 mm) and Ar gas containing O 2 gas were used. A Cu-based wiring film having a thickness of 200 nm was formed by the reactive sputtering used. In addition, as reactive sputtering, it was set as the conditions of the sputtering device of Anelva C-3010, gas pressure 0.5Pa in sputtering atmosphere, and input electric power 1000W. Further, regarding the O 2 partial pressure in the sputtering gas, the film was formed under the condition of 0% for sample 11 and 14% for sample 12.
Each sample measured the specific resistance and measured the X-ray diffraction intensity as in Example 1 to evaluate the peak intensity ratio of Cu and Cu 2 O. Further, the reflectance of the Si film was measured from the glass substrate side with a CM2002 spectrocolorimeter manufactured by Konica Minolta.
Thereafter, heat treatment was performed at 250 ° C. for 1 hour in a vacuum atmosphere in which each sample was decompressed to 100 Pa or less. The specific resistance, X-ray diffraction intensity, and reflectance were also measured for the sample after the heat treatment in the same manner as described above. The results are shown in Table 2.

表２から、本発明例である試料１２では、加熱処理後に比抵抗の上昇がないことからＣｕ系配線膜へのシリコンの拡散反応が生じていないこと分かる。また、配線膜が加熱された際には、Ｃｕがシリコン中へ拡散することによってシリコンが合金化する等の理由から、半透明の薄膜が黒ずむ現象が生じ、シリコン薄膜の反射率が低下する。本発明例の試料１２では、加熱処理後に反射率の低下がないことからシリコン薄膜へのＣｕの拡散反応が生じていないことが確認できる。   From Table 2, it can be seen that in Sample 12 which is an example of the present invention, there is no increase in specific resistance after the heat treatment, and therefore no silicon diffusion reaction occurs in the Cu-based wiring film. Further, when the wiring film is heated, a phenomenon that the semi-transparent thin film is darkened occurs due to the fact that Cu is diffused into the silicon and the silicon is alloyed, and the reflectance of the silicon thin film is lowered. In the sample 12 of the present invention example, it can be confirmed that the Cu diffusion reaction to the silicon thin film does not occur since the reflectance does not decrease after the heat treatment.

また、スパッタリングガス中のＯ２分圧を１２％、投入電力を８００Ｗとする以外は実施例１と同様の条件で、表３に示す各膜厚のＣｕ系配線膜を２５×５０ｍｍのガラス基板上（コーニング１７３７）に成膜した。成膜後の各試料について、実施例１と同様に、比抵抗の測定、ＣｕとＣｕ２Ｏのピーク強度比の評価、密着性試験を行った。その結果を表３に示す。 Further, a Cu-based wiring film having each film thickness shown in Table 3 is a 25 × 50 mm glass substrate under the same conditions as in Example 1 except that the O 2 partial pressure in the sputtering gas is 12% and the input power is 800 W. A film was formed on the top (Corning 1737). For each sample after film formation in the same manner as in Example 1, the measurement of the specific resistance, the evaluation of the peak intensity ratio of Cu and Cu 2 O, the adhesion test was performed. The results are shown in Table 3.

表３から、膜厚１００〜５００ｎｍのＣｕ系配線膜でも、ピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）が０．８〜２．５の範囲であれば十分な密着性を有することが分かる。また、膜厚１００ｎｍの試料２１では、比抵抗が若干高い値となっている。 From Table 3, even with a Cu-based wiring film having a film thickness of 100 to 500 nm, it has sufficient adhesion as long as the peak intensity ratio Cu (111) / Cu 2 O (111) is in the range of 0.8 to 2.5. I understand. Further, in the sample 21 having a film thickness of 100 nm, the specific resistance has a slightly high value.

２５×５０ｍｍのガラス基板上（コーニング１７３７）に、純度９９．９９％のＣｕターゲット（直径１６４ｍｍ×厚さ５ｍｍ）、Ｏ２ガスを含んだＡｒガスを用いた反応性スパッタリングによって、膜厚５０ｎｍのＣｕ系配線膜を成膜した。なお、反応性スパッタリングとしては、アネルバ製Ｃ−３０１０のスパッタリング装置、スパッタリング雰囲気中のガス圧０．５Ｐａ、投入電力８００Ｗの条件とし、スパッタリングガス中のＯ２分圧に関しては１２％の条件で成膜をした。このＣｕ系配線膜をリガク製Ｘ線回折装置ＲＩＮＴ２５００を使用してＸ線回折強度測定を行いＣｕとＣｕ２Ｏのピーク強度比を評価したところ、ピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）＝１．１５であった。 On a 25 × 50 mm glass substrate (Corning 1737), a reactive sputtering using a 99.99% pure Cu target (diameter 164 mm × thickness 5 mm) and Ar gas containing O 2 gas has a thickness of 50 nm. A Cu-based wiring film was formed. Reactive sputtering is performed under the conditions of an Anelva C-3010 sputtering apparatus, a gas pressure in the sputtering atmosphere of 0.5 Pa, and an input power of 800 W, and an O 2 partial pressure in the sputtering gas of 12%. Made a membrane. The Cu-based wiring film was measured for X-ray diffraction intensity using a Rigaku X-ray diffractometer RINT2500 to evaluate the peak intensity ratio of Cu and Cu 2 O. The peak intensity ratio Cu (111) / Cu 2 O ( 111) = 1.15.

続いて、上記のＣｕ系配線膜の上に、純度９９．９９％のＣｕターゲット（直径１６４ｍｍ×厚さ５ｍｍ）、アネルバ製Ｃ−３０１０のスパッタリング装置を用いて、スパッタリング雰囲気中のガス圧０．５Ｐａ、投入電力１２００Ｗの条件とし、スパッタリングガスをＡｒのみとして、膜厚３００ｎｍのＣｕ膜を積層形成した。
上記で作製した積層のＣｕ系配線膜に関して、比抵抗を測定するとともに、密着性試験として積層のＣｕ系配線膜に２ｍｍ間隔で碁盤の目状に切れ目を入れた後、膜表面にテープを貼り、引き剥がした時に基板上に残った桝目を面積率で評価する試験を行った。その結果、比抵抗は２．３μΩｃｍ、密着性は１００％であった。
以上から、積層のＣｕ系配線膜とすることで、密着性と低抵抗特性を両立した配線膜が得られることが分かる。 Subsequently, a Cu target having a purity of 99.99% (diameter: 164 mm × thickness: 5 mm) and an Anelva C-3010 sputtering apparatus are used on the above Cu-based wiring film, and the gas pressure in the sputtering atmosphere is reduced to 0. 0. A Cu film having a film thickness of 300 nm was stacked and formed under the conditions of 5 Pa and input power of 1200 W, using only Ar as the sputtering gas.
Regarding the laminated Cu-based wiring film produced above, the specific resistance was measured and, as an adhesion test, the laminated Cu-based wiring film was cut into a grid pattern at intervals of 2 mm, and then a tape was applied to the film surface. A test was conducted to evaluate the area remaining on the substrate when peeled off by the area ratio. As a result, the specific resistance was 2.3 μΩcm, and the adhesion was 100%.
From the above, it can be seen that by using a laminated Cu-based wiring film, a wiring film having both adhesiveness and low resistance characteristics can be obtained.

Claims (5)

シリコン薄膜直上に形成される、Ｃｕ酸化物を含有する平面表示装置用Ｃｕ系配線膜であって、Ｃｕの主結晶面（１１１）面のＸ線回折ピーク強度をＣｕ（１１１）、Ｃｕ２Ｏの主結晶面（１１１）面のＸ線回折のピーク強度をＣｕ２Ｏ（１１１）とした時に、ピーク強度比Ｃｕ（１１１）／Ｃｕ２Ｏ（１１１）の値が０．８〜２．５の範囲にあることを特徴とする平面表示装置用Ｃｕ系配線膜。 A Cu-based wiring film for a flat panel display device containing Cu oxide and formed immediately above a silicon thin film, wherein the X-ray diffraction peak intensity of the main crystal plane (111) of Cu is Cu (111), Cu 2 O The peak intensity ratio Cu (111) / Cu 2 O (111) is 0.8 to 2.5 when the peak intensity of the X-ray diffraction of the main crystal plane (111) is Cu 2 O (111). A Cu-based wiring film for a flat display device, characterized by being in the range of 前記シリコン薄膜がＳｉウェハ基板上のシリコン薄膜である請求項１に記載の平面表示装置用Ｃｕ系配線膜。 The Cu-based wiring film for a flat display device according to claim 1, wherein the silicon thin film is a silicon thin film on a Si wafer substrate. 膜厚が２００〜５００ｎｍであることを特徴とする請求項１または請求項２に記載の平面表示装置用Ｃｕ系配線膜。   The Cu-based wiring film for a flat panel display device according to claim 1 or 2, wherein the film thickness is 200 to 500 nm. 比抵抗が１５μΩｃｍ以下であることを特徴とする請求項１から請求項３までのいずれか１項に記載の平面表示装置用Ｃｕ系配線膜。   The Cu-based wiring film for a flat panel display device according to any one of claims 1 to 3, wherein a specific resistance is 15 µΩcm or less. 請求項１に記載の平面表示装置用Ｃｕ系配線膜上にＣｕ膜が積層されることを特徴とする平面表示装置用Ｃｕ系配線膜。   A Cu-based wiring film for a flat display device, wherein a Cu film is laminated on the Cu-based wiring film for a flat display device according to claim 1.
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