JPH02301591A - Iron-nickel alloy plating bath - Google Patents
Iron-nickel alloy plating bathInfo
- Publication number
- JPH02301591A JPH02301591A JP12382989A JP12382989A JPH02301591A JP H02301591 A JPH02301591 A JP H02301591A JP 12382989 A JP12382989 A JP 12382989A JP 12382989 A JP12382989 A JP 12382989A JP H02301591 A JPH02301591 A JP H02301591A
- Authority
- JP
- Japan
- Prior art keywords
- plating
- plating bath
- ions
- iron
- malate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000007747 plating Methods 0.000 title claims abstract description 41
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 229940049920 malate Drugs 0.000 claims abstract description 8
- BJEPYKJPYRNKOW-UHFFFAOYSA-N malic acid Chemical compound OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims abstract description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 6
- 239000008139 complexing agent Substances 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 4
- 239000003002 pH adjusting agent Substances 0.000 claims abstract 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- -1 iron ion Chemical class 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 abstract description 5
- 229910052759 nickel Inorganic materials 0.000 abstract description 5
- 229910000889 permalloy Inorganic materials 0.000 abstract description 5
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 2
- 230000000704 physical effect Effects 0.000 abstract description 2
- 239000006174 pH buffer Substances 0.000 abstract 2
- 239000010408 film Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000011790 ferrous sulphate Substances 0.000 description 2
- 235000003891 ferrous sulphate Nutrition 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 2
- 229940081974 saccharin Drugs 0.000 description 2
- 235000019204 saccharin Nutrition 0.000 description 2
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NAOLWIGVYRIGTP-UHFFFAOYSA-N 1,3,5-trihydroxyanthracene-9,10-dione Chemical compound C1=CC(O)=C2C(=O)C3=CC(O)=CC(O)=C3C(=O)C2=C1 NAOLWIGVYRIGTP-UHFFFAOYSA-N 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- 229910020641 Co Zr Inorganic materials 0.000 description 1
- 229910020520 Co—Zr Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- WPUMTJGUQUYPIV-JIZZDEOASA-L disodium (S)-malate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](O)CC([O-])=O WPUMTJGUQUYPIV-JIZZDEOASA-L 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 101150078951 mai-2 gene Proteins 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000019265 sodium DL-malate Nutrition 0.000 description 1
- 239000001394 sodium malate Substances 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野J
本発明は、磁気記録に用いられるパーマロイメッキ液の
浴安定化に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application J] The present invention relates to bath stabilization of permalloy plating solutions used in magnetic recording.
[従来の技術]
従来から、磁気記録用薄膜ヘッド、垂直磁気記録媒体等
に高性能軟磁性材料が使用されている。[Prior Art] High-performance soft magnetic materials have been used for magnetic recording thin film heads, perpendicular magnetic recording media, and the like.
軟磁性材料としては、電気メツキ法によって作られたパ
ーマロイ膜、スパッタ法で作られたパーマロイ膜、セン
ダスト膜、Co−Zr系合金非晶質、蒸着法で作られた
パーマロイ膜等が一般的に用いられている。Commonly used soft magnetic materials include permalloy films made by electroplating, permalloy films made by sputtering, sendust films, amorphous Co-Zr alloys, and permalloy films made by vapor deposition. It is used.
特性的には、内部応力の少ないこと、飽和磁束密度の高
いこと、保持力、異方性磁界の小さいこと、ヒステリシ
ス曲線か理想に近いことなどである。Its characteristics include low internal stress, high saturation magnetic flux density, low coercive force, low anisotropic magnetic field, and close to ideal hysteresis curve.
軟&n性材料の膜厚がある程度要求される場合や量産性
を要求される場合メッキ法が選択されることが多い。The plating method is often selected when a certain level of film thickness of the soft material is required or when mass production is required.
[発明が解決しようとする課題1
しかし、従来技術の鉄ニッケル合金メッキ浴はメッキ液
自身の浴安定性に欠け、沈殿を起こしたり磁気特性の劣
化を起こす等問題点が多かった。[Problem to be Solved by the Invention 1] However, the iron-nickel alloy plating bath of the prior art lacks bath stability of the plating solution itself, and has many problems such as precipitation and deterioration of magnetic properties.
そこで本発明Cまこのような問題点を解決するためのも
ので、その目的とするところは、物性管理がしやすく、
液寿命の長いメッキ浴を提供することにある。Therefore, the present invention C is intended to solve such problems, and its purpose is to easily manage physical properties,
The objective is to provide a plating bath with a long liquid life.
「課−苅を解決するための手段)
本発明は、ニクケルイオン、鉄イオン、これら金属イオ
ンのPH緩衝剤、PH調整剤及び、界面活性剤を含む水
溶液に金属イオンの錯化剤を含むメッキ浴であり、ニッ
ケル、及び、鉄イオンに対して効果的な開化能力を有す
るリンゴ酸塩とクエン酸塩が同時に加えられていること
を特徴としている。"Means for Solving Problems" The present invention provides a plating bath containing a complexing agent for metal ions in an aqueous solution containing Nickel ions, iron ions, a PH buffer for these metal ions, a PH adjuster, and a surfactant. It is characterized by the simultaneous addition of malate and citrate, which have the ability to effectively open up nickel and iron ions.
本発明で、用いられるリンゴ酸塩濃度は、0、I Om
o9/9〜1.Omof2/9.、クエン酸濃度は、O
,lomoI2/42−0.8mo[/eで望ましいリ
ンゴ酸塩1度は、0.30mof2/e〜0.7mo&
/g、、酒石塩濃度は、030moβ/e〜0.6mo
ff/gである。これは、錯化剤濃度が少なすぎると、
本発明の目的とする安定性に欠け、リンゴ酸塩が0.7
moβ/!以上及び、クエン酸塩が0.6moff/f
f以上になった場合は、欲に溶けに(くなる欠点を有す
る。In the present invention, the malate concentration used is 0, I Om
o9/9~1. Omof2/9. , the citric acid concentration is O
, lomoI2/42-0.8mo[/e and the desired malate 1 degree is 0.30mof2/e~0.7mo&
/g, tartaric salt concentration is 030moβ/e~0.6mo
ff/g. This is because if the complexing agent concentration is too low,
It lacks the stability targeted by the present invention, and malate is 0.7
moβ/! above and citrate is 0.6 moff/f
If it exceeds f, it has the disadvantage of becoming greedy.
[作 用1
以上よりメッキ浴の遊離イオンが適切に調節され、メッ
キ被膜の組成が一定に保たれ、又、鉄イオンの酸化によ
る沈殿が防止できることにより液寿命が大巾に向上され
る。[Function 1] From the above, the free ions in the plating bath are appropriately adjusted, the composition of the plating film is kept constant, and precipitation due to oxidation of iron ions can be prevented, thereby greatly improving the life of the solution.
以下、本発明による電気メッキ浴の特徴を比較例及び、
実施例により説明する。Hereinafter, the characteristics of the electroplating bath according to the present invention will be explained as comparative examples and
This will be explained using an example.
〔比 較 例]
銅板を脱脂、水洗、酸浸漬、水洗し、その上に下記のメ
ッキ浴組成およびメッキ条件にて鉄ニッケル合金m性膜
を形成した。[Comparative Example] A copper plate was degreased, washed with water, immersed in acid, and washed with water, and an iron-nickel alloy m-based film was formed thereon using the following plating bath composition and plating conditions.
(メッキ浴組成)
硫酸ニッケル 1.15 mo12/Q塩化
ニッケル 0.10 noβ/eホウ酸
0.24 mo12/Q硫酸第一鉄
0.054 mo12/12サッカリン
0.50 g/f2ラウリル硫酸ナトリウ
ム 0.20 g/ff(メッキ条件)
電流密度・・0.4Adm2
1谷(昌 ・ ・ ・ ・ 35 ℃
PF(・ ・ ・ 2 6以上による条件で60
分メッキし、8μmのメッキ膜を得た。(Plating bath composition) Nickel sulfate 1.15 mo12/Q Nickel chloride 0.10 noβ/e Boric acid
0.24 mo12/Q ferrous sulfate
0.054 mo12/12 saccharin
0.50 g/f2 Sodium lauryl sulfate 0.20 g/ff (plating conditions) Current density...0.4Adm2 1 Valley (Chang ・ ・ ・ ・ 35 ℃
PF (・ ・ ・ 2 60 under the condition of 6 or more
A plating film of 8 μm was obtained.
この膜をVSM測定機で磁気測定をしたところ保持力は
、0.50e、飽和磁束密度は、8000Gであった。When this film was magnetically measured using a VSM measuring device, the coercive force was 0.50e and the saturation magnetic flux density was 8000G.
メッキ浴の安定性に関しては次のようにして確認を行な
った。The stability of the plating bath was confirmed as follows.
銅板(50X50x2mm)を前処理した後、60分メ
ッキして次々にメッキを繰り返した。これを12回繰り
返し、保持力を測定した、その結果を第1図に示す。保
持力は徐々に上昇していく様子がわかる。又、作業終了
後、メッキ浴を観察したところ浴槽の下部に茶色の沈殿
物が確認された。これは、鉄イオンの酸化によるもので
、保持力の上昇原因と考えられる。After pre-treating a copper plate (50x50x2mm), it was plated for 60 minutes and plating was repeated one after another. This was repeated 12 times and the holding force was measured. The results are shown in FIG. It can be seen that the holding power gradually increases. Furthermore, when the plating bath was observed after the work was completed, a brown precipitate was observed at the bottom of the bath. This is due to the oxidation of iron ions and is thought to be the cause of the increase in retention.
又、本店では、40℃以上にすると、鉄イオン酸化が急
激に進み、磁気特性かでないことが確認された。In addition, at our head office, we have confirmed that when the temperature is above 40°C, iron ion oxidation rapidly progresses, causing the magnetic properties to deteriorate.
以上の結果により、磁気特性が不安定で、浴寿命が、非
常に短いことが判明した。The above results revealed that the magnetic properties were unstable and the bath life was extremely short.
[実施例11
下記の組成のメッキ浴を用いて比較例と同様の方法で鉄
ニッケル合金磁性膜を形成した6(メッキ浴組成)
1iiif M ニッケル 1.15 mo
!!、/12 ’塩化ニッケル 0.10
mail/12ホウ酸 0.24
mo(2/E硫酸第一鉄 0゜054
mog/シ11ンゴ酸ナトリウム 0.50’ m
ap!/Eクエン酸ナトリウム 0.40 moQ
/Qサッカリン 0.50 g/ff
ラウリル硫酸ナトリウム 020 g/I2比較例と
同様に磁気特性を調べたところ一回目のメッキ膜は°、
保持力0130eで飽和磁束密度は、8200Gであっ
た。[Example 11 An iron-nickel alloy magnetic film was formed in the same manner as in the comparative example using a plating bath with the following composition 6 (Plating bath composition) 1iiiif M Nickel 1.15 mo
! ! , /12' Nickel chloride 0.10
mail/12 boric acid 0.24
mo(2/E ferrous sulfate 0°054
mog/sodium cylinlate 0.50' m
ap! /E Sodium citrate 0.40 moQ
/Q Saccharin 0.50 g/ff
Sodium lauryl sulfate 020 g/I2 When the magnetic properties were investigated in the same manner as the comparative example, the first plating film was °;
The saturation magnetic flux density was 8200G at a coercive force of 0130e.
又、メッキ浴の安定性に関しては第2図に示すように保
持力は、非常に安定した経緯を示した。Regarding the stability of the plating bath, as shown in FIG. 2, the holding force showed a very stable history.
その後、−日おきに、−回メツキを行ないこれを−か月
間繰り返した6結果は良好で、安定した保持力を示し、
浴槽に沈殿物は確認されなかった。After that, plating was carried out once every -day and this was repeated for -6 months.The results were good, showing stable holding power.
No sediment was found in the bathtub.
さらに1本店組成で、80℃まで上昇させたが泪は安定
状態を保った。Furthermore, with one main store composition, the temperature remained stable even though the temperature was raised to 80°C.
以上の結果により1M1気特性がきわめて安定でしかも
液寿命も非常に長いことが確認された。From the above results, it was confirmed that the 1M1 gas characteristics are extremely stable and the liquid life is also extremely long.
[実 施 例 2]
本発明の鉄ニッケル合金メッキ浴を装飾、防食メッキと
して検討した。[Example 2] The iron-nickel alloy plating bath of the present invention was studied as a decorative and anticorrosive plating.
(メジキン谷組成)
硫酸ニッケル 0.40 mol/シ塩化ニ
ッケル 0.25 mo12/g。(Mejikin valley composition) Nickel sulfate 0.40 mol/Nickel silchloride 0.25 mol/g.
ホウ酸 0.75 maI2/12疏
酸第−9失 0. 03
5 mol/12リンゴ酸ナトリウム 0.50
moβ/εクエン酸ナトリウム 0.35
mo9!/12サッカリン 0.50
g/Qラウリル硫酸ナトリウム 0.20g/n(
メッキ条件)
電流密度=0.4Adm”
(6温・・・・35℃ P)l・・・2.6真鍮性の
時計ケースを前処理し上記メッキ条件で5umのメッキ
を施した。Boric acid 0.75 maI2/12 saccharic acid No.9 loss 0. 03
5 mol/12 sodium malate 0.50
moβ/ε Sodium citrate 0.35
mo9! /12 Saccharin 0.50
g/Q Sodium lauryl sulfate 0.20g/n (
Plating conditions) Current density = 0.4 Adm" (6 temperature...35°C P) l...2.6 A brass watch case was pretreated and plated to a thickness of 5 um under the above plating conditions.
その結果、この合金メッキは光沢と平滑性にすぐれ、高
い装飾効果が得られた。As a result, this alloy plating had excellent gloss and smoothness, and a high decorative effect was obtained.
又、メッキ被膜中の鉄分の含有率は約25%でアノード
金属のコストダウンに役立つほか、メッキ?&Ilφが
延展性に冨もため各種製品への応用展開が可能であるこ
とがわかった。In addition, the iron content in the plating film is approximately 25%, which helps reduce the cost of the anode metal. It was found that &Ilφ has excellent spreadability and can be applied to various products.
[発明の効果]
以上、述べてきたように本発明の鉄ニッケル合金メッキ
浴により、長期に渡り安定した&nn時特性メッキ性、
及び、良質なメッキ膜が得られることが可能になった。[Effects of the Invention] As described above, the iron-nickel alloy plating bath of the present invention provides stable plating properties over a long period of time,
Moreover, it became possible to obtain a high-quality plating film.
第1図は、比較例で用いたメッキ浴における浴のめっき
回数と保持力の変化を示す図である。
第2図は、実施例で用いたメッキ浴における浴のめっき
回数と保持力の変化を示す図である。
以上FIG. 1 is a diagram showing the change in the number of plating times and the holding force of the plating bath used in the comparative example. FIG. 2 is a diagram showing changes in the number of times of plating and the holding force in the plating bath used in Examples. that's all
Claims (1)
緩衝剤、PH調整剤及び、界面活性剤を含む水溶液に前
記金属イオンの錯化剤としてリンゴ酸塩、及び、クエン
酸塩を含むことを特徴とする鉄ニッケル合金メッキ浴。Nickel ion, iron ion, pH of these metal ions
An iron-nickel alloy plating bath characterized in that an aqueous solution containing a buffer, a pH adjuster, and a surfactant contains malate and citrate as complexing agents for the metal ions.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP12382989A JPH02301591A (en) | 1989-05-17 | 1989-05-17 | Iron-nickel alloy plating bath |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP12382989A JPH02301591A (en) | 1989-05-17 | 1989-05-17 | Iron-nickel alloy plating bath |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH02301591A true JPH02301591A (en) | 1990-12-13 |
Family
ID=14870398
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP12382989A Pending JPH02301591A (en) | 1989-05-17 | 1989-05-17 | Iron-nickel alloy plating bath |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH02301591A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5897692A (en) * | 1996-09-10 | 1999-04-27 | Denso Corporation | Electroless plating solution |
JP2011168831A (en) * | 2010-02-18 | 2011-09-01 | Kyoto Ichi | Method for manufacturing iron-nickel alloy plating film having high hardness and low thermal expansion coefficient |
-
1989
- 1989-05-17 JP JP12382989A patent/JPH02301591A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5897692A (en) * | 1996-09-10 | 1999-04-27 | Denso Corporation | Electroless plating solution |
JP2011168831A (en) * | 2010-02-18 | 2011-09-01 | Kyoto Ichi | Method for manufacturing iron-nickel alloy plating film having high hardness and low thermal expansion coefficient |
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