JP5572815B2 - Method and device for forming iron having corrosion resistance - Google Patents
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- JP5572815B2 JP5572815B2 JP2012242104A JP2012242104A JP5572815B2 JP 5572815 B2 JP5572815 B2 JP 5572815B2 JP 2012242104 A JP2012242104 A JP 2012242104A JP 2012242104 A JP2012242104 A JP 2012242104A JP 5572815 B2 JP5572815 B2 JP 5572815B2
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims description 116
- 229910052742 iron Inorganic materials 0.000 title claims description 48
- 238000005260 corrosion Methods 0.000 title claims description 20
- 230000007797 corrosion Effects 0.000 title claims description 20
- 238000000034 method Methods 0.000 title claims description 18
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 239000010409 thin film Substances 0.000 description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001420 photoelectron spectroscopy Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
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Description
本発明は、材料の表面改質法に係り、とくに、鉄表面に酸化鉄層を形成することによる耐食性を有する鉄の形成法及びそれを用いたデバイスに関する。 The present invention relates to a surface modification method of a material, and more particularly to a method of forming iron having corrosion resistance by forming an iron oxide layer on an iron surface and a device using the same.
鉄は、強磁性、耐熱性、資源的に豊富であるなど優れた特性を有しているため、バルクのみならず薄膜としての利用も望まれている。しかし、鉄は耐食性に欠けるため、その利用の範囲は制限されてきた。 Since iron has excellent properties such as ferromagnetism, heat resistance, and abundant resources, it is desired to be used not only as a bulk but also as a thin film. However, since iron lacks corrosion resistance, the range of its use has been limited.
そのため、錆びにくい鉄を形成するための手法の確立が課題となっている。 Therefore, establishment of the technique for forming iron which does not rust easily has been an issue.
そこで、本発明は、上記の点に鑑み、高い耐食性を有する、つまり錆にくい鉄を形成することが可能な耐食性を有する鉄の形成法及びそれを用いたデバイスを提供することを目的とする。 Therefore, in view of the above points, an object of the present invention is to provide a method of forming iron having high corrosion resistance, that is, having corrosion resistance capable of forming iron that is not easily rusted, and a device using the same.
本発明の第１の態様は耐食性を有する鉄の形成法であり、酸素を含む雰囲気中における波長２００ｎｍ以下の光照射により、純鉄表面に酸化鉄層としてのＦｅ３Ｏ４層を形成することを特徴とする。 The first aspect of the present invention is a method for forming corrosion-resistant iron, and an Fe 3 O 4 layer as an iron oxide layer is formed on a pure iron surface by light irradiation with a wavelength of 200 nm or less in an atmosphere containing oxygen. It is characterized by.
本発明の第２の態様も耐食性を有する鉄の形成法であり、酸素を含む雰囲気中における波長２００ｎｍ以下の光照射により、鉄表面に含まれる炭素を除去し、かつ酸化鉄層としてのＦｅ３Ｏ４層を形成することを特徴とする。 The second aspect of the present invention is also a method for forming corrosion-resistant iron, in which carbon contained in the iron surface is removed by irradiation with light having a wavelength of 200 nm or less in an oxygen-containing atmosphere , and Fe 3 as an iron oxide layer. An O 4 layer is formed.
本発明の第３の態様はデバイスであり、第１又は第２の態様に係る鉄の形成法で得られた耐食性を有する鉄を備えることを特徴とする。 A third aspect of the present invention is a device, comprising iron having corrosion resistance obtained by the iron forming method according to the first or second aspect.
なお、以上の構成要素の任意の組合せ、本発明の表現を方法やシステムなどの間で変換したものもまた、本発明の態様として有効である。 It should be noted that any combination of the above-described constituent elements, and those obtained by converting the expression of the present invention between methods and systems are also effective as aspects of the present invention.
本発明によれば、高い耐食性を有する鉄の形成手法を確立でき、鉄材料を使用することで高い性能を発揮できるデバイス作製の基礎技術として利用可能であるなど、あらゆる分野において必要不可欠な技術となる。 According to the present invention, it is possible to establish a method for forming iron having high corrosion resistance, and it can be used as a basic technology for device fabrication that can exhibit high performance by using an iron material. Become.
以下、図面を参照しながら本発明の好適な実施の形態を詳述する。なお、各図面に示される同一または同等の構成要素、部材、処理等には同一の符号を付し、適宜重複した説明は省略する。また、実施の形態は発明を限定するものではなく例示であり、実施の形態に記述されるすべての特徴やその組み合わせは必ずしも発明の本質的なものであるとは限らない。 Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings. In addition, the same code | symbol is attached | subjected to the same or equivalent component, member, process, etc. which are shown by each drawing, and the overlapping description is abbreviate | omitted suitably. In addition, the embodiments do not limit the invention but are exemplifications, and all features and combinations thereof described in the embodiments are not necessarily essential to the invention.
図１で本発明に係る耐食性を有する鉄の形成法の実施の形態を示す。図１（ａ）では、板状もしくは薄膜状の純鉄１の表面に、波長２００ｎｍ以下の光としてレーザー光２を酸素を含む雰囲気中（例えば大気中乃至減圧空気中あるいは酸素のみの雰囲気中等であり、圧力は大気圧以下とは限らない）にて照射する。図１（ｂ）には、レーザー光照射により鉄表面に形成された酸化鉄（Ｆｅ３Ｏ４）層３が示されている。前記薄膜状の純鉄１は基板上に真空蒸着等で形成可能である。なお、波長２００ｎｍより波長の長い光は酸素分子に吸収されなくなるため、有効ではない。
FIG. 1 shows an embodiment of a method for forming iron having corrosion resistance according to the present invention. In FIG. 1A, the surface of a
図１において、純鉄の代わりに、炭素を含む低純度の鉄材料を用いてもよい。また、板状もしくは薄膜状の鉄の代わりに、粒子状など別の形態の鉄材料を用いてもよい。 In FIG. 1, a low-purity iron material containing carbon may be used instead of pure iron. Further, instead of plate-like or thin-film iron, other forms of iron material such as particles may be used.
この耐食性を有する鉄の形成法で得られた鉄を備えたデバイスは、例えば、所定の基板上に薄膜状の純鉄１を真空蒸着等で形成後、前記レーザー光の照射を行って表面に酸化鉄（Ｆｅ３Ｏ４）層を形成することで得られる。これにより基板上に耐食性鉄薄膜を有する磁性体デバイスが得られる。必要に応じて、基板上に他の薄膜や素子を形成すればよい。
A device provided with iron obtained by this method of forming iron having corrosion resistance is formed on a surface by, for example, forming thin-film
この実施の形態によれば、次の通りの効果を得ることができる。 According to this embodiment, the following effects can be obtained.
(1) 純鉄にレーザー光２を照射する場合、純鉄の表面に極薄い緻密な酸化鉄（Ｆｅ３Ｏ４）層を形成できる。 (1) When irradiating laser light 2 to pure iron, an extremely thin dense iron oxide (Fe 3 O 4 ) layer can be formed on the surface of pure iron.
(2) 炭素を含む低純度の鉄材料を用いる場合、レーザー光２の照射によって鉄表面に含まれる炭素を除去し、かつ極薄い緻密な酸化鉄（Ｆｅ３Ｏ４）層を形成できる。 (2) When a low-purity iron material containing carbon is used, the carbon contained in the iron surface can be removed by irradiation with laser light 2 and an extremely thin dense iron oxide (Fe 3 O 4 ) layer can be formed.
(3) 耐食性を有する鉄を備えるデバイスを作製可能である。 (3) It is possible to produce a device comprising iron having corrosion resistance.
以下、本発明に係る耐食性を有する鉄の形成法を実施例で詳述する。 Hereinafter, the method for forming corrosion-resistant iron according to the present invention will be described in detail in Examples.
スライドガラス基板上（大きさ８×２６ｍｍ２、厚さ１ｍｍ）に、鉄板（純度９９.９９％）をターゲットとした電子ビーム蒸着法により、純鉄薄膜（膜厚５０ｎｍ）を形成した。その試料表面に、波長１５７ｎｍのフッ素（Ｆ２）レーザー光を照射した。そのときの単一パルス当たりのレーザーフルエンスは４０ｍＪ／ｃｍ２、パルス繰り返し周波数は１０Ｈｚ、照射時間は６０ｍｉｎとした。また、レーザー光のパルス幅は２０ｎｓであった。レーザー光照射は室温、大気圧中で行った。
A pure iron thin film (film thickness 50 nm) was formed on a slide glass substrate (size 8 × 26 mm 2 ,
Ｆ２レーザー光が照射された試料表面の化学結合状態を、光電子分光分析により調べた。Ｆ２レーザー光が照射されたＦｅ薄膜の最表面において、７１０.８ｅＶにＦｅ２Ｏ３を示すピークが測定された。このピークは、レーザー光未照射の試料表面でも見られることから、自然酸化によるものと考えられる。その後、試料をＡｒ＋イオンスパッタリング（加速電圧２ｋＶ）により深さ方向に分析を進めていくと、表面から深さ１ｎｍのところでは、ピークの位置が７１０.４ｅＶに化学シフトすることがわかった。これは、Ｆｅ３Ｏ４層の形成を示している。また、深さ３ｎｍでは、Ｆｅ単体を示すピーク（７０７.０ｅＶ）が見え始めた。したがって、約１ｎｍ厚のＦ２Ｏ３自然酸化層の下に、Ｆ２レーザー光の照射により、約２ｎｍ厚のＦｅ３Ｏ４層が形成していることが判明した。 The chemical bonding state of the sample surface irradiated with the F 2 laser beam was examined by photoelectron spectroscopy. A peak indicating Fe 2 O 3 at 710.8 eV was measured on the outermost surface of the Fe thin film irradiated with the F 2 laser beam. Since this peak is also observed on the surface of the sample not irradiated with laser light, it is considered that this peak is due to natural oxidation. Thereafter, when the sample was analyzed in the depth direction by Ar + ion sputtering (acceleration voltage 2 kV), it was found that the peak position was chemically shifted to 710.4 eV at a depth of 1 nm from the surface. This indicates the formation of the Fe 3 O 4 layer. Further, at a depth of 3 nm, a peak (707.0 eV) indicating Fe alone began to appear. Therefore, it was found that an Fe 3 O 4 layer having a thickness of about 2 nm was formed under the F 2 O 3 natural oxide layer having a thickness of about 1 nm by irradiation with F 2 laser light.
レーザー光未照射及び照射試料を用いて、アノード分極挙動による耐食性試験を行った。試験では、対極にＰｔ板を使用し、参照電極としてＡｇ／ＡｇＣｌを用いた。測定における印加電圧の走査速度は１.７５ｍＶ／ｓとした。試験溶液には、模擬海水として、濃度３ｗｔ％のＮａＣｌ水溶液を用いた。未照射試料の場合、自然電位が約−６８０ｍＶであったが、Ｆ２レーザー光照射後、約−３１５ｍＶまで変化し、３６５ｍＶ程度移行することが認められた。また、未照射試料に比べて照射試料では、電圧印加後０.０５ｍＡ／ｃｍ２までは勾配が緩やかであった。その後、未照射試料と同じ勾配で直線的に変化した。以上より、Ｆ２レーザー光により形成したＦｅ３Ｏ４層は、ＮａＣｌ水溶液中での電圧印加によっても、Ｆｅ薄膜からＦｅイオンの溶出を著しく抑制することがわかった。したがって、Ｆ２レーザー光により、耐食性を呈するＦｅ薄膜の形成が可能となった。 A corrosion resistance test based on anodic polarization behavior was performed using the laser light unirradiated and irradiated samples. In the test, a Pt plate was used as the counter electrode, and Ag / AgCl was used as the reference electrode. The scanning speed of the applied voltage in the measurement was 1.75 mV / s. The test solution used was a 3 wt% NaCl aqueous solution as simulated seawater. In the case of the unirradiated sample, the natural potential was about −680 mV, but after irradiation with the F 2 laser light, it changed to about −315 mV, and a shift of about 365 mV was observed. In addition, compared with the unirradiated sample, the gradient of the irradiated sample was gentle until 0.05 mA / cm 2 after voltage application. Thereafter, it changed linearly with the same gradient as the unirradiated sample. From the above, it has been found that the Fe 3 O 4 layer formed by the F 2 laser beam remarkably suppresses the elution of Fe ions from the Fe thin film even when a voltage is applied in an NaCl aqueous solution. Therefore, it became possible to form an Fe thin film exhibiting corrosion resistance by F 2 laser light.
Ｆ２レーザー光が照射された試料を、濃度０.０１ｗｔ％のＨＮＯ３水溶液中に６０ｍｉｎ浸漬した結果、耐薬品性を呈することがわかった。また、濃度３ｗｔ％のＮａＣｌ水溶液中において３日間浸漬しても、Ｆ２レーザー光が照射された試料表面では錆びは発生しなかった。 As a result of immersing the sample irradiated with the F 2 laser beam in an aqueous HNO 3 solution having a concentration of 0.01 wt% for 60 min, it was found that the sample exhibited chemical resistance. Further, even when immersed in a 3 wt% NaCl aqueous solution for 3 days, no rust was generated on the surface of the sample irradiated with the F 2 laser beam.
純鉄薄膜の代わりに鋳鉄板を用い、その表面に波長１５７ｎｍのＦ２レーザー光を照射した。そのときの単一パルス当たりのレーザーフルエンスは４０ｍＪ／ｃｍ２、パルス繰り返し周波数は１０Ｈｚ、照射時間は６０ｍｉｎとした。また、レーザー光のパルス幅は２０ｎｓであった。レーザー光照射は室温、大気圧中で行った。 A cast iron plate was used instead of the pure iron thin film, and the surface thereof was irradiated with F 2 laser light having a wavelength of 157 nm. The laser fluence per single pulse at that time was 40 mJ / cm 2 , the pulse repetition frequency was 10 Hz, and the irradiation time was 60 min. The pulse width of the laser light was 20 ns. Laser light irradiation was performed at room temperature and atmospheric pressure.
Ｆ２レーザー光が照射された試料表面の化学結合状態を、光電子分光分析により調べた。Ｆ２レーザー光の照射後、炭素を示すピーク（２８４.５ｅＶ）が見られなくなった。また、Ｆ２レーザー光照射後約２ｎｍのＦｅ３Ｏ４層の形成も認められた。したがって、鉄表面に含まれる炭素がＦ２レーザー光の照射により除去され、純化した表面が酸化鉄（Ｆｅ３Ｏ４）層に改質されたものと考えられる。 The chemical bonding state of the sample surface irradiated with the F 2 laser beam was examined by photoelectron spectroscopy. After irradiation with F 2 laser light, a peak indicating carbon (284.5 eV) was not observed. Moreover, formation of a Fe 3 O 4 layer of about 2 nm after F 2 laser light irradiation was also observed. Therefore, it is considered that carbon contained in the iron surface was removed by irradiation with F 2 laser light, and the purified surface was modified into an iron oxide (Fe 3 O 4 ) layer.
上記実施例で述べたように、本発明によれば、高い耐食性を有する鉄が形成できるようになり、鉄材料を使用することで高い性能を発揮できるデバイスの作製に繋がる。この結果は、電気電子工学分野でのデバイス作製の基礎技術に適用可能になるなど、その用途はあらゆる分野で有用である。 As described in the above embodiments, according to the present invention, iron having high corrosion resistance can be formed, and the use of an iron material leads to the production of a device capable of exhibiting high performance. This result is useful in all fields, such as being applicable to basic technology for device fabrication in the field of electrical and electronic engineering.
以上、実施の形態及び実施例を例に本発明を説明したが、実施の形態の各構成要素や各処理プロセスには請求項に記載の範囲で種々の変形が可能であることは当業者に理解されるところである。以下、変形例について触れる。 Although the present invention has been described above by way of embodiments and examples, it will be understood by those skilled in the art that various modifications can be made to each component and each processing process of the embodiments within the scope of the claims. It is understood. Hereinafter, modifications will be described.
実施例では、鉄表面に波長１５７ｎｍのフッ素（Ｆ２）レーザー光を照射する場合で説明したが、Ｏ２を分解できる波長２００ｎｍ以下（とくに好ましくは波長１５７ｎｍ以下）の光照射であれば、同等の効果が期待できる。また、照射する光はレーザー光であってもよいし、それ以外の光であってもよい。 In the examples, the case where the iron surface is irradiated with a fluorine (F 2 ) laser beam having a wavelength of 157 nm has been described. However, if light irradiation with a wavelength of 200 nm or less (particularly preferably, wavelength of 157 nm or less) that can decompose O 2 is used, Can be expected. Further, the light to be irradiated may be laser light or other light.
１ 板状もしくは薄膜状の純鉄
２ レーザー光
３ 酸化鉄（Ｆｅ３Ｏ４）層
1 Plate-like or thin-film pure iron 2 Laser light 3 Iron oxide (Fe 3 O 4 ) layer
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