JP3852446B2 - Resistance thin film material and method of manufacturing resistance thin film using the same - Google Patents
Resistance thin film material and method of manufacturing resistance thin film using the same Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims description 59
- 239000000463 material Substances 0.000 title claims description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 16
- 238000005477 sputtering target Methods 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000011810 insulating material Substances 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000011651 chromium Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 229910021364 Al-Si alloy Inorganic materials 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910018487 Ni—Cr Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910001122 Mischmetal Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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Description
本発明は、電子部品に用いられる抵抗薄膜材料、抵抗薄膜形成用のスパッタリングターゲット、およびこのスパッタリングターゲットを用いた抵抗薄膜の製造方法に関する。 The present invention relates to a resistance thin film material used for an electronic component, a sputtering target for forming a resistance thin film, and a method of manufacturing a resistance thin film using the sputtering target.
チップ抵抗器、精密抵抗器、ネットワーク抵抗器、高圧抵抗器などの抵抗器、測温抵抗体、感温抵抗器などの温度センサ、および、ハイブリットＩＣとその複合モジュール製品などの電子部品には、抵抗薄膜を使用した薄膜抵抗器が用いられている。 Electronic components such as chip resistors, precision resistors, network resistors, resistors such as high-voltage resistors, temperature sensors such as resistance temperature detectors, temperature sensitive resistors, and hybrid IC and its composite module products Thin film resistors using resistive thin films are used.
この薄膜抵抗器においては、多くの場合、抵抗薄膜材料としてＴａ金属、ＴａＮ化合物、Ｎｉ−Ｃｒ合金が用いられており、中でもＮｉ−Ｃｒ合金が最も一般的に用いられている。 In this thin film resistor, Ta metal, TaN compound, and Ni—Cr alloy are often used as the resistive thin film material, and Ni—Cr alloy is most commonly used among them.
薄膜抵抗材料を含むすべての抵抗材料では、その使用にあたって、高温（１５５℃程度）において抵抗変化率が小さく非常に安定であること、すなわち、高温安定性と抵抗温度係数（ＴＣＲ）とが重要な特性となる。一般に、ＮｉおよびＣｒのみからなる２元系合金の場合は、Ｎｉ／Ｃｒの比を変え、高温安定性と抵抗温度係数（ＴＣＲ）の制御を行う。しかし、高温において抵抗値が安定であることと抵抗温度係数（ＴＣＲ）がほぼ０であることを同時に実現することは困難である。そのため、特許第２５４２５０４号公報、特開平６−２０８０３号公報に記載されるように、Ｎｉ−Ｃｒ−Ａｌ−Ｓｉ合金とすることにより特性の改善が検討されてきた。 In all resistive materials including thin film resistive materials, the resistance change rate is small and very stable at high temperature (about 155 ° C.), that is, high temperature stability and resistance temperature coefficient (TCR) are important. It becomes a characteristic. In general, in the case of a binary alloy composed only of Ni and Cr, the Ni / Cr ratio is changed to control the high temperature stability and the resistance temperature coefficient (TCR). However, it is difficult to simultaneously realize that the resistance value is stable at a high temperature and that the temperature coefficient of resistance (TCR) is almost zero. Therefore, as described in Japanese Patent No. 2542504 and Japanese Patent Laid-Open No. 6-20803, improvement of characteristics has been studied by using a Ni—Cr—Al—Si alloy.
しかしながら、近年、自動車などに搭載される薄膜抵抗器では、使用環境温度の上昇に伴い、抵抗特性、特に高温安定性に対する要求がさらにレベルアップしてきている。従来よりさらに使用温度が高い１７５℃程度において抵抗変化率が小さく、同時に抵抗温度係数（ＴＣＲ）がほぼ０であることが要求されるようになってきたが、前述の薄膜抵抗材料でも、このように厳格な要求に応えることができていない。 However, in recent years, with respect to thin film resistors mounted on automobiles and the like, the requirement for resistance characteristics, particularly high-temperature stability, has further increased as the operating environment temperature rises. It has been demanded that the rate of change in resistance is small at a temperature of about 175 ° C., which is higher than the conventional temperature, and at the same time the temperature coefficient of resistance (TCR) is almost zero. To meet strict requirements.
本発明は、これまでのＮｉ−Ｃｒ系合金の中でも優れた高温安定性を有するとされていたＮｉ−Ｃｒ−Ａｌ−Ｓｉ系合金よりもさらに優れた高温安定性を得ることと、抵抗温度係数（ＴＣＲ）をほぼ０とすることとを、同時に実現する抵抗薄膜材料を提供することを目的とする。 The present invention has a higher temperature stability than the Ni-Cr-Al-Si alloy, which has been considered to have excellent high temperature stability among the conventional Ni-Cr alloys, and has a resistance temperature coefficient. An object of the present invention is to provide a resistance thin film material that simultaneously realizes that (TCR) is substantially zero.
また、かかる抵抗薄膜材料を用いた抵抗薄膜形成用のスパッタリングターゲット、このスパッタリングターゲットを用いた抵抗薄膜およびその製造方法を提供する。 Moreover, the sputtering target for resistance thin film formation using this resistance thin film material, the resistance thin film using this sputtering target, and its manufacturing method are provided.
本発明の抵抗薄膜材料は、Ａｌ：１〜１５質量％、希土類元素：０．０１〜０．５質量％を含み、残部が実質的にＣｒ／Ｎｉ比が質量で０．１５〜１．１となるＣｒおよびＮｉからなることを特徴とする。本発明における希土類元素としては、Ｙおよびランタノイド（典型的にはランタン、セリウム）があげられるが、これらの中から１種または２種以上を選び、添加することができる。また、セリウム族希土類元素の混合物であるミッシュメタルを使用することもできる。 The resistance thin film material of the present invention contains Al: 1 to 15% by mass, rare earth element: 0.01 to 0.5% by mass, and the balance is substantially 0.15 to 1.1 by mass in Cr / Ni ratio. It consists of Cr and Ni which become. Examples of the rare earth element in the present invention include Y and lanthanoids (typically lanthanum and cerium), and one or more of them can be selected and added. Misch metal which is a mixture of cerium group rare earth elements can also be used.
上記の抵抗薄膜材料から薄膜抵抗器用の抵抗薄膜を得るには、Ｎｉ−Ｃｒ−Ａｌ−希土類元素合金スパッタリングターゲットを使用する。その組成は、前記抵抗薄膜材料と実質的に同じである。 In order to obtain a resistance thin film for a thin film resistor from the above resistance thin film material, a Ni—Cr—Al—rare earth element alloy sputtering target is used. Its composition is substantially the same as that of the resistive thin film material.
かかるスパッタリングターゲットを用いて、スパッタ法により、絶縁材料基板上に、Ｎｉ−Ｃｒ−Ａｌ−希土類元素合金からなる抵抗薄膜を生成させる。なお、その組成は、前記抵抗薄膜材料と実質的に同じである。その後、該抵抗薄膜が形成された基板を、大気中において、温度２００℃〜５００℃で、１〜１０時間、熱処理を行うことにより抵抗薄膜を完成する。かかる抵抗薄膜を用いることで、高温での抵抗変化率が小さく、同時に抵抗温度係数（ＴＣＲ）がほぼ０である薄膜抵抗器を得ることができる。 Using such a sputtering target, a resistance thin film made of a Ni—Cr—Al—rare earth element alloy is formed on an insulating material substrate by sputtering. The composition is substantially the same as that of the resistive thin film material. Thereafter, the substrate on which the resistance thin film is formed is heat-treated at a temperature of 200 ° C. to 500 ° C. for 1 to 10 hours in the air to complete the resistance thin film. By using such a resistance thin film, it is possible to obtain a thin film resistor having a small resistance change rate at a high temperature and simultaneously having a resistance temperature coefficient (TCR) of almost zero.
本発明の組成範囲において真空中で成膜されたままの抵抗薄膜は、抵抗温度係数が負に大きく、また高温における抵抗安定性が不十分である。しかしながら、本発明に係る熱処理を行うことにより、当該抵抗薄膜の抵抗温度係数を安定的に±１０ｐｐｍ以内とすることができる。また、薄膜表面に緻密な酸化膜が形成され、高温で安定な抵抗薄膜が得られる。かかる抵抗薄膜を用いた薄膜抵抗器は、従来のＮｉ−Ｃｒ−Ａｌ−Ｓｉ系合金でも実現することができなかった抵抗特性が得られ、その結果、厳しい高温環境下で使用される電子部品に適するという顕著な効果が得られる。 The resistive thin film as it is deposited in a vacuum in the composition range of the present invention has a negative resistance temperature coefficient that is negatively large and has insufficient resistance stability at high temperatures. However, by performing the heat treatment according to the present invention, the resistance temperature coefficient of the resistance thin film can be stably within ± 10 ppm. In addition, a dense oxide film is formed on the surface of the thin film, and a resistive thin film that is stable at high temperatures can be obtained. A thin film resistor using such a resistance thin film has a resistance characteristic that could not be realized even with a conventional Ni-Cr-Al-Si alloy, and as a result, it can be used as an electronic component used in a severe high temperature environment. The remarkable effect of being suitable is obtained.
本発明の抵抗薄膜材料は、Ｃｒ／Ｎｉ比が質量で０．１５〜１．１であるＮｉ−Ｃｒ合金に、Ａｌを１〜１５質量％、希土類元素を０．０１〜０．５質量％、それぞれ添加したものである。 The resistance thin film material of the present invention is a Ni-Cr alloy having a Cr / Ni ratio of 0.15 to 1.1 by mass, Al of 1 to 15 mass%, and a rare earth element of 0.01 to 0.5 mass%. , Respectively.
Ｃｒ／Ｎｉ比が質量で０．１５未満であると、抵抗温度係数が大きくなってしまう。一方、１．１を超えると、１７５℃における抵抗変化率が高くなり、高温安定性を損なってしまう。 If the Cr / Ni ratio is less than 0.15 by mass, the temperature coefficient of resistance increases. On the other hand, if it exceeds 1.1, the rate of change in resistance at 175 ° C. becomes high, and high-temperature stability is impaired.
Ａｌは、主として抵抗温度係数（ＴＣＲ）を改善するために添加する。その添加量が１質量％未満であるか、または１５質量％を超えると、抵抗温度係数（ＴＣＲ）は負に大きくなってしまい、高温安定性も悪化してしまう。 Al is mainly added to improve the temperature coefficient of resistance (TCR). When the addition amount is less than 1% by mass or exceeds 15% by mass, the temperature coefficient of resistance (TCR) becomes negatively large and the high temperature stability is also deteriorated.
希土類元素は、本明細書では、Ｙとランタノイドを意味し、主として高温安定性を改善するために添加する。その添加量が０．０１質量％未満であると、高温安定性の改善に寄与しない。一方、０．５質量％を超えても、高温安定性に格別の効果増大が期待できず、コストアップとなるので、好ましくない。 In the present specification, the rare earth element means Y and a lanthanoid, and is added mainly to improve high-temperature stability. If the addition amount is less than 0.01% by mass, it does not contribute to the improvement of high temperature stability. On the other hand, if it exceeds 0.5% by mass, it cannot be expected that a significant effect on high-temperature stability will be increased, resulting in an increase in cost.
本発明に係る抵抗薄膜は、次のようにして製造する。Ｎｉ−Ｃｒ−Ａｌ−希土類元素を特定の組成範囲内で調整して作製したスパッタリングターゲットを用いて、スパッタ法により、絶縁材料基板上に抵抗薄膜を成膜し、その後、この基板を大気中において、温度２００℃〜５００℃で、１〜１０時間、熱処理を行う。 The resistive thin film according to the present invention is manufactured as follows. Using a sputtering target prepared by adjusting Ni-Cr-Al-rare earth elements within a specific composition range, a resistive thin film was formed on an insulating material substrate by sputtering, and then the substrate was placed in the atmosphere. The heat treatment is performed at a temperature of 200 ° C. to 500 ° C. for 1 to 10 hours.
熱処理温度が、２００℃未満であると、抵抗温度係数（ＴＣＲ）が安定しない。一方、５００℃を超えると、抵抗温度係数（ＴＣＲ）が大きくなってしまう。 When the heat treatment temperature is less than 200 ° C., the temperature coefficient of resistance (TCR) is not stable. On the other hand, when it exceeds 500 ° C., the temperature coefficient of resistance (TCR) becomes large.
また、熱処理時間が、１時間未満であると、抵抗温度係数（ＴＣＲ）が安定しない。一方、１０時間を超えても、抵抗安定性に対する効果の増大はみられず、コストアップとなり好ましくない。 Further, if the heat treatment time is less than 1 hour, the temperature coefficient of resistance (TCR) is not stable. On the other hand, even if it exceeds 10 hours, the increase in the effect on the resistance stability is not seen, and the cost increases, which is not preferable.
（実施例１〜２４、比較例１〜１３）
まず、電気ニッケル、電解クロム、アルミニウムメタルショット、Ｙメタル（試薬）、Ｌａメタル（試薬）、Ｃｅメタル（試薬）、ミッシュメタル（試薬）、金属シリコン塊（試薬）を原料とし、表１および表２に示す組成となるようにそれぞれ秤量して、真空溶解炉により、約２ｋｇのＮｉ−Ｃｒ−Ａｌ−希土類合金およびＮｉ−Ｃｒ−Ａｌ−Ｓｉ合金のインゴットを作製した。
(Examples 1-24, Comparative Examples 1-13)
First, using nickel, electrolytic chromium, aluminum metal shot, Y metal (reagent), La metal (reagent), Ce metal (reagent), misch metal (reagent), and metal silicon lump (reagent), Table 1 and Table Each was weighed so as to have the composition shown in FIG. 2, and ingots of about 2 kg of Ni—Cr—Al—rare earth alloy and Ni—Cr—Al—Si alloy were prepared in a vacuum melting furnace.
次に、抵抗薄膜を製造するために、それぞれのインゴットを、均質化処理の後、ワイヤカットで厚さ５ｍｍ、直径１５０ｍｍの丸板を切り出し、上下面を研削してターゲットとした。 Next, in order to manufacture a resistance thin film, each ingot was homogenized, and then a round plate having a thickness of 5 mm and a diameter of 150 mm was cut by wire cutting, and the upper and lower surfaces were ground to obtain targets.
成膜工程は、カソードスパッタ法によって、以下のように行った。真空室にアルミナ基板を装入し、１×１０-4Ｐａに排気した後、純度９９．９９９５％のアルゴンガスを導入して０．３Ｐａの圧力に保ち、スパッタパワー０．３ｋＷで、膜厚が５００Åとなるように前記基板上に成膜を行った。 The film forming process was performed by cathode sputtering as follows. An alumina substrate was charged into the vacuum chamber and evacuated to 1 × 10 −4 Pa. Then, argon gas having a purity of 99.9995% was introduced and maintained at a pressure of 0.3 Pa, and the sputtering power was 0.3 kW. The film was formed on the substrate so as to be 500 mm.
得られた抵抗薄膜の両側に、膜厚５０００ÅのＡｕ電極を、同様にカソードスパッタ法により成膜し、アルミナ基板上に抵抗薄膜およびＡｕ電極が形成された薄膜抵抗器を得た。その後、大気中、３００℃で、３時間の熱処理を行うことにより、それぞれの薄膜抵抗器を完成した。 An Au electrode having a film thickness of 5000 mm was similarly formed on both sides of the obtained resistance thin film by the cathode sputtering method to obtain a thin film resistor having a resistance thin film and an Au electrode formed on an alumina substrate. Then, each thin film resistor was completed by performing the heat processing for 3 hours at 300 degreeC in air | atmosphere.
なお、成膜法としては、カソードスパッタ法の他に、電子ビームや抵抗加熱式蒸着法などを用いることもできる。 In addition to the cathode sputtering method, an electron beam, a resistance heating vapor deposition method, or the like can be used as the film forming method.
このようにして作製した実施例１〜２４および比較例１〜１３の薄膜抵抗器について、抵抗温度係数（ＴＣＲ）を評価するため、恒温槽で昇温しながら抵抗測定を行い、２５℃と１２５℃における抵抗温度係数（ＴＣＲ）を測定した。また、高温安定性は、次のように評価した。それぞれの薄膜抵抗器を、１７５℃の恒温槽内に、２０００時間保持し、その保持の前後で抵抗値を測定し、抵抗変化率を測定した。その結果を表１および表２に示す。 In order to evaluate the resistance temperature coefficient (TCR) of the thin film resistors of Examples 1 to 24 and Comparative Examples 1 to 13 manufactured in this way, resistance measurement was performed while raising the temperature in a thermostatic bath. The temperature coefficient of resistance (TCR) at 0 ° C. was measured. The high temperature stability was evaluated as follows. Each thin film resistor was held in a thermostatic bath at 175 ° C. for 2000 hours, the resistance value was measured before and after the holding, and the resistance change rate was measured. The results are shown in Tables 1 and 2.
実施例１〜２４の薄膜抵抗器は、いずれも抵抗温度係数（ＴＣＲ）ほぼ０で、±２５ｐｐｍ／℃の範囲にあり、良好な抵抗温度係数（ＴＣＲ）を示した。また、実施例１〜２４の薄膜抵抗器は、いずれも１７５℃における抵抗変化率が０．１０％未満であり、主な従来技術のＮｉ−Ｃｒ−Ａｌ−Ｓｉ合金である比較例１３と比較しても、きわめて高い高温安定性を示した。 The thin film resistors of Examples 1 to 24 all had a temperature coefficient of resistance (TCR) of almost 0 and were in a range of ± 25 ppm / ° C., and exhibited a good temperature coefficient of resistance (TCR). Further, the thin film resistors of Examples 1 to 24 all have a resistance change rate at 175 ° C. of less than 0.10%, and are compared with Comparative Example 13 which is a Ni—Cr—Al—Si alloy of the main prior art. Even so, it showed very high temperature stability.
図１に、実施例５、比較例３、５、１３の抵抗薄膜から製造した薄膜抵抗器の抵抗変化率の推移を、図２に、実施例１７および比較例１３の抵抗薄膜から製造した薄膜抵抗器の抵抗変化率の推移をグラフで示した。 FIG. 1 shows the change in resistance change rate of the thin film resistors manufactured from the resistive thin films of Example 5 and Comparative Examples 3, 5, and 13. FIG. 2 shows the thin film manufactured from the resistive thin films of Example 17 and Comparative Example 13. The transition of the resistance change rate of the resistor is shown in a graph.
Claims (4)
A thin film made of a Ni—Cr—Al—rare earth alloy is formed on an insulating material substrate by a sputtering method using the sputtering target according to claim 2, and then the substrate on which the resistive thin film is formed is exposed to the atmosphere. A method for producing a resistance thin film, wherein heat treatment is performed at a temperature of 200 ° C. to 500 ° C. for 1 to 10 hours.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004006981A JP3852446B2 (en) | 2003-11-04 | 2004-01-14 | Resistance thin film material and method of manufacturing resistance thin film using the same |
| CNB2004100900571A CN1321206C (en) | 2003-11-04 | 2004-11-01 | Metal resistor material, sputtering target material, resistor film and their manufactures |
| TW93133312A TWI250218B (en) | 2003-11-04 | 2004-11-02 | Metallic resistance material, sputtering target, resistance thin film, and method for making the resistance thin film |
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| JP2003374063 | 2003-11-04 | ||
| JP2004006981A JP3852446B2 (en) | 2003-11-04 | 2004-01-14 | Resistance thin film material and method of manufacturing resistance thin film using the same |
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| JP2005154884A JP2005154884A (en) | 2005-06-16 |
| JP3852446B2 true JP3852446B2 (en) | 2006-11-29 |
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| JP4622522B2 (en) * | 2005-01-07 | 2011-02-02 | 住友金属鉱山株式会社 | Metal resistor material, resistance thin film, sputtering target, thin film resistor, and manufacturing method thereof |
| JP2014241451A (en) * | 2014-09-18 | 2014-12-25 | 住友金属鉱山株式会社 | Resistance thin film element with copper conductor layer |
| KR101848764B1 (en) | 2016-04-15 | 2018-04-19 | 한국에너지기술연구원 | Micro temperature sensor and fabrication method of the same |
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