JP4190973B2 - Method for producing cobalt-platinum alloy magnetic film by electrodeposition - Google Patents
Method for producing cobalt-platinum alloy magnetic film by electrodeposition Download PDFInfo
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- 238000004070 electrodeposition Methods 0.000 title claims description 29
- GUBSQCSIIDQXLB-UHFFFAOYSA-N cobalt platinum Chemical compound [Co].[Pt].[Pt].[Pt] GUBSQCSIIDQXLB-UHFFFAOYSA-N 0.000 title claims description 25
- 229910001260 Pt alloy Inorganic materials 0.000 title claims description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 238000007747 plating Methods 0.000 claims description 37
- 239000010941 cobalt Substances 0.000 claims description 22
- 229910017052 cobalt Inorganic materials 0.000 claims description 22
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 22
- 238000000137 annealing Methods 0.000 claims description 11
- WLQXLCXXAPYDIU-UHFFFAOYSA-L cobalt(2+);disulfamate Chemical compound [Co+2].NS([O-])(=O)=O.NS([O-])(=O)=O WLQXLCXXAPYDIU-UHFFFAOYSA-L 0.000 claims description 8
- IXSUHTFXKKBBJP-UHFFFAOYSA-L azanide;platinum(2+);dinitrite Chemical compound [NH2-].[NH2-].[Pt+2].[O-]N=O.[O-]N=O IXSUHTFXKKBBJP-UHFFFAOYSA-L 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- 239000010408 film Substances 0.000 description 66
- 238000000034 method Methods 0.000 description 12
- 239000013078 crystal Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910020707 Co—Pt Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 1
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
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Description
本発明は、磁気記録媒体を構成する磁性膜の形成に関し、特に、コバルト−白金合金（以下、単にＣｏ−Ｐｔ合金と略す場合もある）磁性膜を電析法によるめっき膜により形成する技術に関する。 The present invention relates to the formation of a magnetic film constituting a magnetic recording medium, and more particularly, to a technique for forming a cobalt-platinum alloy (hereinafter, also simply abbreviated as Co-Pt alloy) magnetic film by a plating film by an electrodeposition method. .
近年、磁気記録媒体の製造においては、記録密度の高密度化のため、スパッタリング法や真空蒸着法のような乾式法によりディスク基板上に形成した磁性膜を記録層とする薄膜型の磁気記録媒体の研究開発が盛んに行われている。 In recent years, in the manufacture of magnetic recording media, in order to increase the recording density, a thin-film magnetic recording medium using a magnetic film formed on a disk substrate by a dry method such as a sputtering method or a vacuum evaporation method as a recording layer Research and development is actively conducted.
この磁気記録媒体の磁性膜材料としては、コバルトを含むコバルト系合金が一般的に知られている。これらの磁性膜は高記録密度特性等の優れた磁気特性を有し、例えば、乾式法により形成した薄膜の記録層はその記録密度を飛躍的に向上させているのが現状である。 As a magnetic film material of this magnetic recording medium, a cobalt-based alloy containing cobalt is generally known. These magnetic films have excellent magnetic characteristics such as high recording density characteristics. For example, the recording density of a thin recording layer formed by a dry method has dramatically improved the recording density.
しかしながら、乾式法により磁性膜を形成する場合、大量生産性の観点からすると、十分に満足するものとはいえない。いわゆるブロードバンド化による大量情報通信技術の進展や小型モータ、マイクロマシンなどの開発を考慮すると、今後、高密度の記録媒体や優れた磁気特性を有する素材は必須であり、大量且つ低コストで磁性膜を提供できる製造技術が必要となる。このようなことから、大量生産が可能となる電析めっきという湿式法による磁性膜製造技術が現在注目されている。 However, when forming a magnetic film by a dry method, it cannot be said that it is fully satisfied from the viewpoint of mass productivity. Considering the progress of mass information communication technology by so-called broadband and the development of small motors, micromachines, etc., high-density recording media and materials with excellent magnetic properties will be essential in the future. Manufacturing technology that can be provided is required. For these reasons, a magnetic film manufacturing technique based on a wet method called electrodeposition plating that enables mass production is now drawing attention.
このコバルト−白金合金磁性膜としては、例えばＣｏ−Ｐｔ合金磁性膜形成用のめっき浴が知られている（特許文献１参照）。 As this cobalt-platinum alloy magnetic film, for example, a plating bath for forming a Co-Pt alloy magnetic film is known (see Patent Document 1).
このコバルト−白金合金磁性膜は原子組成比が１：１である場合、高密度の磁気記録媒体への応用としての可能性があり、近年特に注目されている。それは、Ｃｏ−Ｐｔ合金磁性膜が通常不規則なｆｃｃ構造をとっているものの、６００〜７００℃付近で熱処理を行うと、ＡｕＣｌ型、Ｌ１０のｆｃｔ構造の規則構造となり、高い一軸結晶磁気異方性を有するためである。 When the atomic composition ratio of the cobalt-platinum alloy magnetic film is 1: 1, there is a possibility of application to a high-density magnetic recording medium. It although Co-Pt alloy magnetic film is normally taken irregular fcc structure, when subjected to heat treatment at around 600 to 700 ° C., AuCl type becomes the ordered structure of the fct structure L1 0, high uniaxial crystal magnetic anisotropy This is because it has a directivity.
しかしながら、現状知られている電析法により得られたコバルト−白金合金磁性膜は、その磁気特性、より具体的には磁気の強さを示す保磁力が十分なものとは言えない。特に、乾式法で得られたコバルト−白金合金磁性膜に比較すると、実用上十分に満足できる保磁力を有するものが得られないことが指摘されている。 However, a cobalt-platinum alloy magnetic film obtained by a currently known electrodeposition method cannot be said to have sufficient magnetic properties, more specifically, a coercive force indicating a magnetic strength. In particular, it has been pointed out that, compared with a cobalt-platinum alloy magnetic film obtained by a dry method, a film having a coercive force sufficiently satisfactory for practical use cannot be obtained.
本発明は、以上のような事情のもとになされたもので、電析によりコバルト−白金合金めっき膜を形成し、種々の検討を行った結果、従来の電析によるめっき膜では実現できなかったレベルの高保持力を有するコバルト−白金合金磁性膜を得ることができることを見出し、本発明を想到するに至った。 The present invention has been made under the circumstances as described above. As a result of forming a cobalt-platinum alloy plating film by electrodeposition and conducting various studies, it cannot be realized by a conventional plating film by electrodeposition. It has been found that a cobalt-platinum alloy magnetic film having a high level of holding power can be obtained, and the present invention has been conceived.
本発明は、ジニトロジアンミン白金を２ｍＭと、アミドスルホン酸コバルトを１〜５ｍＭと、クエン酸アンモニウムを２０ｍＭとを含有し、ｐＨ７．５〜８．０に調整された電析めっき浴から電析により形成されるコバルト−白金合金磁性膜の製造方法において、電析して得られたコバルト−白金めっき被膜に、６００〜８００℃の焼鈍処理を行うものである。 The present invention comprises 2 mM dinitrodiammine platinum, 1 to 5 mM cobalt amidosulfonate, and 20 mM ammonium citrate by electrodeposition from an electrodeposition plating bath adjusted to pH 7.5 to 8.0. In the method for producing a cobalt-platinum alloy magnetic film to be formed, a cobalt-platinum plating film obtained by electrodeposition is subjected to an annealing treatment at 600 to 800 ° C.
本発明により得られたコバルト−白金合金磁性膜は、本発明者らの知る限りにおいて、電析により得られためっき膜の中で最大の保持力が実現できたものである。例えば、非特許文献１によれば、電析めっき膜により、保持力４８３ｋＡ／ｍのコバルト−白金合金磁性膜が実現できたことが報告されているが、本発明に係るコバルト−白金合金磁性膜の製造方法によれば、この非特許文献１に比較すると、約２倍の保持力、即ち、約８８０ｋＡ／ｍもの高保持力を有するコバルト−白金合金磁性膜を得ることができる。
As far as the present inventors know, the cobalt-platinum alloy magnetic film obtained by the present invention can realize the maximum holding force among the plated films obtained by electrodeposition. For example, according to Non-Patent
本発明に係るコバルト−白金合金磁性膜の製造方法では、ジニトロジアンミン白金と、アミドスルホン酸コバルトと、クエン酸アンモニウムとを含有し、ｐＨ７．５〜９．０に調整された電析めっき浴から電析により形成することができる。 In the method for producing a cobalt-platinum alloy magnetic film according to the present invention, from an electrodeposition plating bath containing dinitrodiammine platinum, cobalt amidosulfonate, and ammonium citrate and adjusted to pH 7.5 to 9.0. It can be formed by electrodeposition.
このような本発明に係るコバルト−白金合金磁性膜形成用の電析めっき浴により磁性膜を形成する場合、液温５０〜８０℃でめっき処理を行うことが好ましい。 When the magnetic film is formed by such an electrodeposition plating bath for forming a cobalt-platinum alloy magnetic film according to the present invention, the plating treatment is preferably performed at a liquid temperature of 50 to 80 ° C.
本発明に係るコバルト−白金合金磁性膜形成用の電析めっき浴によりめっき膜を形成した後は、得られる磁性膜を６００〜８００℃の焼鈍処理を行う。この焼鈍処理は、減圧雰囲気中、例えば３×１０−３Ｐａ、１０〜９０分間の熱処理を行うことが好ましい。 After the plating film is formed by the electrodeposition plating bath for forming a cobalt-platinum alloy magnetic film according to the present invention, the obtained magnetic film is annealed at 600 to 800 ° C. The annealing treatment is preferably performed in a reduced pressure atmosphere, for example, 3 × 10 −3 Pa, for 10 to 90 minutes.
以上説明したように、本発明に係るのコバルト−白金合金磁性膜の製造方法によれば、従来の電析法による磁性膜では実現できないレベルの優れた磁気特性を備えるコバルト−白金合金磁性膜を製造すること可能となる。 As described above, according to the method of manufacturing a cobalt-platinum alloy magnetic film according to the present invention, a cobalt-platinum alloy magnetic film having excellent magnetic properties that cannot be achieved by a magnetic film formed by a conventional electrodeposition method is provided. It becomes possible to manufacture.
以下に、本発明の好ましい実施の形態に実施例に基づいて説明する。 Hereinafter, preferred embodiments of the present invention will be described based on examples.
本実施例は、以下に示す組成の電析めっき浴を用い、コバルト含有率の異なるめっき膜を形成し、各めっき膜の結晶構造、磁気特性を調べた結果を説明する。 In this example, the results of examining the crystal structure and the magnetic characteristics of each plating film by forming plating films having different cobalt contents using an electrodeposition plating bath having the following composition will be described.
電析めっき浴は、ジニトロジアンミン白金は２ｍＭ（０．６４ｇ／Ｌ）と、クエン酸アンモニウムは２０ｍＭ（４．１６ｇ／Ｌ）とを含有し、アミドスルホン酸コバルトの濃度を変化させたものを使用した。アミドスルホン酸コバルト濃度は、１ｍＭ、２ｍＭ、３ｍＭ、４ｍＭ、５ｍＭ（０．２５〜１．２５ｇ／Ｌ）とすることで、コバルト含有率が異なる５種類の組成のコバルト−白金合金めっき膜を形成した。電析めっき条件は、Ａｇ／ＡｇＣｌ（参照電極）を基準に基板電位−１Ｖとし、液温６０℃、ｐＨ８．０（水酸化ナトリウム使用）とした。被めっき対象物はＩＴＯ基材（透明電極基材）を用い、アノードとして白金シートを用いた。図１に、アミドスルホン酸コバルトの濃度とめっき膜のコバルト含有率の関係を示したグラフを示す。尚、コバルト含有率は、ＥＤＸ分析装置により特定した。 The electrodeposition plating bath uses dinitrodiammine platinum containing 2 mM (0.64 g / L), ammonium citrate containing 20 mM (4.16 g / L), and varying the concentration of cobalt amidosulfonate. did. The cobalt amidosulfonate concentration is 1 mM, 2 mM, 3 mM, 4 mM, and 5 mM (0.25 to 1.25 g / L), thereby forming cobalt-platinum alloy plating films having five different compositions with different cobalt contents. did. The electrodeposition conditions were a substrate potential of -1 V based on Ag / AgCl (reference electrode), a liquid temperature of 60 ° C., and a pH of 8.0 (using sodium hydroxide). As the object to be plated, an ITO base material (transparent electrode base material) was used, and a platinum sheet was used as an anode. FIG. 1 is a graph showing the relationship between the concentration of cobalt amidosulfonate and the cobalt content of the plating film. The cobalt content was specified by an EDX analyzer.
図１を見ると判るように、電析めっき浴中のアミドスルホン酸コバルト濃度が増加するに伴って、得られためっき膜のコバルト含有率は２４ａｔ％、３４ａｔ％、４３ａｔ％、５０ａｔ％、５７ａｔ％と増加していることを確認した。 As can be seen from FIG. 1, as the cobalt amidosulfonate concentration in the electrodeposition plating bath increases, the cobalt content of the obtained plating film is 24 at%, 34 at%, 43 at%, 50 at%, 57 at. % And increased.
次に、コバルト含有率が異なる５種類の各めっき膜についての結晶構造をＸ線回折により調べた結果について説明する。結晶構造は、ＣｕＫαのＸ線回折により、電析直後の各めっき膜と、赤外炉（３×１０−３Ｐａ）中、８００℃、９０分間の焼鈍処理を行った、焼鈍処理後の各めっき膜とについて調査した。その結果を図２に示す。 Next, the results of examining the crystal structure of each of the five types of plating films having different cobalt contents by X-ray diffraction will be described. Each crystal structure was subjected to annealing treatment at 800 ° C. for 90 minutes in each plated film immediately after electrodeposition and in an infrared furnace (3 × 10 −3 Pa) by X-ray diffraction of CuKα. The plating film was investigated. The result is shown in FIG.
図２中、白丸で示したものが電析直後のめっき膜の結果である。電析直後のめっき膜においては、不規則化ｆｃｃ構造の特徴を示すＸ線回折ピークが観察された。また、電析直後のめっき膜では、コバルト含有率の増加に伴い格子定数の数値減少を示す傾向が判明した。この傾向は、図２中破線で示しているべガード則の関係と一致するものであった。この結果より、電析直後のめっき膜は、コバルト−白金の固溶体を形成していることが確認された。 In FIG. 2, what is indicated by white circles is the result of the plated film immediately after electrodeposition. In the plated film immediately after electrodeposition, an X-ray diffraction peak indicating the characteristics of the disordered fcc structure was observed. In addition, it was found that the plating film immediately after electrodeposition tends to show a numerical decrease in the lattice constant as the cobalt content increases. This tendency coincided with the relationship of the Vegard law indicated by the broken line in FIG. From this result, it was confirmed that the plating film immediately after electrodeposition formed a cobalt-platinum solid solution.
図２中、黒四角、白四角で示したものが焼鈍処理後のめっき膜であり、黒四角がａ−軸格子定数のもので、白四角がｃ−軸格子定数の測定結果である。Ｘ線回折により、Ｌ１０相のｆｃｔ配向の形成を示す（００１）、（１１０）の超格子ピークは、コバルト含有率２４ａｔ％〜５７ａｔ％の焼鈍処理後のめっき膜において観察された。また、図２で示すようにｆｃｔ相のａ−軸格子定数は、コバルト含有率には依存せずに、約３．８０Åであることが判明した。そして、ｆｃｔ相のｃ−軸格子定数は、コバルト含有率の増加に伴い、格子定数の数値減少の傾向を示すことが判明した。さらに、コバルト含有率５０ａｔ％の焼鈍処理後のめっき膜においては、ｃ／ａ比率が０．９７にもなり、この数値はバルクでの数値（０．９６８）に匹敵するものであることが判明した。 In FIG. 2, black squares and white squares are the plated films after annealing, the black squares are the a-axis lattice constants, and the white squares are the c-axis lattice constant measurement results. The X-ray diffraction, shows the formation of fct orientation of L1 0 phase (001), the superlattice peak of (110) was observed in the plating film after the annealing process the cobalt content of 24at% ~57at%. Further, as shown in FIG. 2, the a-axis lattice constant of the fct phase was found to be about 3.80% without depending on the cobalt content. And it became clear that the c-axis lattice constant of the fct phase shows a tendency for the numerical value of the lattice constant to decrease as the cobalt content increases. Furthermore, in the plated film after the annealing treatment with a cobalt content of 50 at%, the c / a ratio was 0.97, which was found to be comparable to the bulk value (0.968). did.
コバルト含有率５７ａｔ％の焼鈍処理後のめっき膜においては、（００１）、（１１０）の超格子ピークはその強度も弱く、ブロードとなっていた。そして、Ｌ１０相のｆｃｔ配向の形成を対応して現れる（２００）、（００２）の屈折による特徴的なピークは観察されなかった。このことにより、コバルト含有率５７ａｔ％の焼鈍処理のめっき膜では、規則、不規則変態が非常に困難なものであると考えられた。 In the plated film after the annealing treatment with a cobalt content of 57 at%, the superlattice peaks of (001) and (110) were weak in intensity and broad. No characteristic peak due to refraction of (200) and (002) appearing corresponding to the formation of the Lct 0 phase fct alignment was observed. Thus, it was considered that regular and irregular transformations were very difficult in the annealed plating film having a cobalt content of 57 at%.
続いて、各めっき膜の磁気特性を調べた結果について説明する。磁気特性測定は、上記Ｘ線回折をした各めっき膜について行った。この磁気特性は、振動型磁気天秤（ＶＳＭ）により、７〜８Ｔの正磁場下における磁化の強さを測定したものである。図３には、焼鈍処理後のめっき膜における保磁力を示す。図示は省略するが、電析直後のめっき膜では、１５〜４４ｋＡ／ｍの低い保磁力しか測定されなかった。しかしながら、図３に示すように、コバルト含有率３４ａｔ％〜５０ａｔ％のめっき膜については、焼鈍処理を行うと、著しく保磁力が向上していることが判明した。 Then, the result of having investigated the magnetic characteristic of each plating film is demonstrated. The magnetic characteristics were measured for each plated film subjected to the X-ray diffraction. This magnetic property is obtained by measuring the strength of magnetization under a positive magnetic field of 7 to 8 T using a vibration type magnetic balance (VSM). FIG. 3 shows the coercive force in the plated film after the annealing treatment. Although illustration is omitted, only a low coercive force of 15 to 44 kA / m was measured in the plated film immediately after electrodeposition. However, as shown in FIG. 3, it was found that the coercive force of the plated film having a cobalt content of 34 at% to 50 at% was remarkably improved when annealing was performed.
そして、本実施例におけるめっき膜では、その保磁力がコバルト含有率に大きく依存し、コバルト含有率４３ａｔ％において最大８８１ｋＡ／ｍの保磁力を達成することが判明した。この最大数値は、バルクの場合と同じレベルの保磁力であり、本発明者らの知る電析によるコバルト−白金合金めっき膜の磁性膜の中で、最も大きな値である。このように非常に高い保磁力を有するコバルト−白金合金めっき膜の磁性膜が得られたのは、ｃ／ａ比率０．９７〜０．９８もの、高い磁気結晶異方性を有しためっき膜であることに起因するものと推定される。 And in the plating film in a present Example, it turned out that the coercive force largely depends on cobalt content rate, and achieves the coercive force of 881 kA / m at the maximum in cobalt content rate 43at%. This maximum value is the same level of coercive force as in the case of the bulk, and is the largest value among the magnetic films of the cobalt-platinum alloy plating film obtained by electrodeposition as known by the present inventors. A cobalt-platinum alloy plating film having a very high coercive force was obtained as a plating film having a c / a ratio of 0.97 to 0.98 and a high magnetic crystal anisotropy. This is presumed to be due to the fact that
また、図３中には、ヒステリシス曲線（ＭＨ曲線）の一部を示しているが、コバルト含有率３４ａｔ％、５０ａｔ％のめっき膜では軟磁性相の存在があることが認められた。この軟磁性相は不規則相の残存によるものと推定された。 FIG. 3 shows a part of the hysteresis curve (MH curve), and it was recognized that a soft magnetic phase was present in the plated film having a cobalt content of 34 at% and 50 at%. This soft magnetic phase was assumed to be due to the remaining irregular phase.
Claims (1)
電析して得られたコバルト−白金合金めっき膜に、６００〜８００℃の焼鈍処理を行うことを特徴とするコバルト−白金系磁性膜の製造方法。
Cobalt formed by electrodeposition from an electrodeposition plating bath containing 2 mM dinitrodiammine platinum, 1 to 5 mM cobalt amidosulfonate, and 20 mM ammonium citrate and adjusted to pH 7.5 to 9.0. -In the method of manufacturing a platinum alloy magnetic film,
A method for producing a cobalt-platinum-based magnetic film, comprising subjecting a cobalt-platinum alloy plating film obtained by electrodeposition to an annealing treatment at 600 to 800 ° C.
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