WO2020079977A1 - 表面処理液及びニッケル含有材料の表面処理方法 - Google Patents
表面処理液及びニッケル含有材料の表面処理方法 Download PDFInfo
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- WO2020079977A1 WO2020079977A1 PCT/JP2019/034713 JP2019034713W WO2020079977A1 WO 2020079977 A1 WO2020079977 A1 WO 2020079977A1 JP 2019034713 W JP2019034713 W JP 2019034713W WO 2020079977 A1 WO2020079977 A1 WO 2020079977A1
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- nickel
- surface treatment
- containing material
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- treatment liquid
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/50—Treatment of iron or alloys based thereon
Definitions
- the present invention relates to a surface treatment liquid used for treating the surface of a nickel-containing material, and a surface treatment method for a nickel-containing material using the same. More specifically, the present invention relates to a surface treatment liquid used for treating the surface of an Invar material such as Fe—Ni 36% or the like, or a nickel-containing material such as austenitic stainless steel, and a surface treatment method of the nickel-containing material using the same.
- an Invar material such as Fe—Ni 36% or the like
- a nickel-containing material such as austenitic stainless steel
- the Invar material has a small coefficient of thermal expansion, and thus is suitably used for these parts and the like.
- a technique is known in which a metal material having a resist pattern is processed by a wet etching method to form a fine line.
- fine powdery foreign matter called “smut” may be formed on the surface of the metal material, and the adhesion between the metal material and the resist pattern may be reduced. Therefore, a method has been developed in which the surface of a metal material is treated with a surface treatment liquid to suppress the formation of smut and improve the adhesion between the metal material and the resist pattern.
- Patent Document 1 discloses a surface treatment agent containing hydrogen peroxide, a mineral acid, azoles, silver ions, and halogen ions as a surface treatment agent for improving the adhesion between a copper-plated substrate and a dry film resist.
- Patent Document 2 discloses a surface treatment agent for copper or copper alloy containing a nitrogen-containing heterocyclic compound and an acid such as an inorganic acid or an organic acid.
- Patent Documents 1 and 2 were effective to some extent for copper. However, even if these surface treatment agents are applied to nickel-containing materials such as Invar material and austenitic stainless steel, it is difficult to suppress the formation of smuts. It was not possible to improve the adhesion. If the adhesion between the substrate such as a nickel-containing material and the resist pattern is low, the resist pattern is likely to be peeled off, and it becomes difficult to form fine wiring according to the resist pattern. Therefore, there has been a demand for a surface treatment liquid capable of suppressing the formation of smut and improving the adhesion between the nickel-containing material and the resist pattern.
- the present invention has been made to solve the above problems, and its object is to suppress the formation of smut when etching a nickel-containing material and to improve the adhesion between the resist pattern and the nickel-containing material. It is an object of the present invention to provide a surface treatment liquid for a nickel-containing material that can improve Another object of the present invention is to provide a surface treatment method for a nickel-containing material using the above surface treatment liquid.
- a nickel-containing material surface treatment liquid which is an aqueous solution containing specific components, can solve the above-mentioned problems, and arrived at the present invention.
- a surface treatment liquid for treating the surface of a nickel-containing material which comprises (A) ferric ion 0.05 to 5 mass%; (B) inorganic acid 0.5 to 20 1% to 20% by mass of (C) at least one compound selected from the group consisting of triammonium citrate, ammonium lactate, ammonium formate, diammonium hydrogen citrate, ammonium glycolate, and ammonium malate; and A surface treatment liquid that is an aqueous solution containing water is provided.
- a surface treatment method for a nickel-containing material which comprises a step of bringing the surface treatment liquid into contact with the surface of the nickel-containing material.
- a surface treatment liquid for a nickel-containing material which is capable of suppressing the formation of a smut when etching a nickel-containing material and improving the adhesion between a resist pattern and the nickel-containing material. You can Further, according to the present invention, it is possible to provide a surface treatment method for a nickel-containing material using the surface treatment liquid.
- nickel-containing material in the present specification refers to a metal material containing at least 1% by mass of nickel.
- nickel-containing material for example, nickel simple substance; Fe-Ni 36%, Fe-Ni 32% -Co 5%, Fe-Ni 29% -Co 17%, Fe-Ni 42% -Cr-Ti, Ni-Mo 28% -Fe 2%, etc.
- Low thermal expansion iron-nickel alloy also called invar material
- austenitic stainless steel such as SUS301, SUS304, SUS316
- copper-nickel alloy such as white copper, nickel silver; nickel-titanium alloy; nickel-zinc alloy; nickel-chromium alloy A nickel-cobalt alloy or the like
- the nickel-containing material to be the surface treated body the above-mentioned Invar material or stainless steel is preferable, and the Invar material is particularly preferable.
- a surface treatment liquid which is an embodiment of the present invention, is a liquid composition for treating the surface of a nickel-containing material, and comprises (A) ferric ion 0.05 to 5 mass%; and (B) an inorganic acid. 0.5 to 20 mass%; (C) at least one compound 1 to 3 selected from the group consisting of triammonium citrate, ammonium lactate, ammonium formate, diammonium hydrogen citrate, ammonium glycolate, and ammonium malate 20% by mass; and an aqueous solution containing water.
- the surface treatment liquid contains (A) ferric ion (hereinafter, also referred to as “(A) component”).
- the component (A) may be any compound that can supply (generate) ferric ion into the surface treatment liquid.
- An iron (III) compound can be used as a source of ferric ion. Examples of the iron (III) compound include iron (III) chloride, iron (III) bromide, iron (III) iodide, iron (III) sulfate, iron (III) nitrate, and iron (III) acetate. Can be mentioned.
- iron (III) chloride and iron (III) sulfate are preferable, and iron (III) sulfate is particularly preferable, because the formation of smut can be suppressed more effectively.
- the source of the component (A) may be an anhydride or a hydrate.
- the concentration of the component (A) in the surface treatment liquid is 0.05 to 5% by mass, preferably 0.1 to 3% by mass, and more preferably 0.2 to 1% by mass.
- the concentration of the component (A) means the concentration of ferric ion.
- the concentration of the component (A) is about 2.8% by mass. If the concentration of the component (A) is less than 0.05% by mass, the time required for the surface treatment will be extremely long and the productivity will be reduced. On the other hand, if the concentration of the component (A) exceeds 5% by mass, it becomes difficult to suppress the formation of smut.
- the surface treatment liquid contains (B) an inorganic acid (hereinafter, also referred to as “(B) component”).
- the component (B) include sulfuric acid, nitric acid, boric acid, and hydrogen chloride.
- sulfuric acid and hydrogen chloride are preferable, and sulfuric acid is particularly preferable, because the effect of suppressing the formation of smut is high.
- the sulfuric acid may be either concentrated sulfuric acid or diluted sulfuric acid. Commercially available sulfuric acid can be used as it is or after being appropriately diluted.
- the source of hydrogen chloride may be either concentrated hydrochloric acid or diluted hydrochloric acid. Commercially available hydrochloric acid can be used as it is or after being appropriately diluted.
- the concentration of the component (B) in the surface treatment liquid is 0.5 to 20% by mass, preferably 1 to 10% by mass, more preferably 1 to 5% by mass.
- concentration of the component (B) is less than 0.5% by mass, the time required for the surface treatment becomes very long, and the productivity is reduced.
- concentration of the component (B) exceeds 20% by mass, it becomes difficult to suppress the formation of smut.
- the surface treatment liquid is (C) at least one compound selected from the group consisting of triammonium citrate, ammonium lactate, ammonium formate, diammonium hydrogen citrate, ammonium glycolate, and ammonium malate (hereinafter, “( C) component ").
- component (C) a commercially available product can be used.
- triammonium citrate is particularly preferable because it has a high effect of suppressing the formation of smut.
- the concentration of the component (C) in the surface treatment liquid is 1 to 20% by mass, preferably 2 to 17% by mass, more preferably 3 to 15% by mass. If the concentration of the component (C) is less than 1% by mass, the effect of suppressing the formation of smut cannot be sufficiently obtained. On the other hand, even if the concentration of the component (C) exceeds 20 mass%, the effect obtained by blending the component (C) is not improved so much, and it becomes difficult to dissolve the component (C).
- the surface treatment liquid further contains (D) formic acid (hereinafter, also referred to as “(D) component”).
- (D) component formic acid
- the concentration of the component (D) in the surface treatment liquid is preferably 0.05 to 5% by mass, more preferably 0.1 to 3% by mass, and 0.2 to 1% by mass. Is particularly preferable.
- concentration of the component (D) is less than 0.05% by mass, the effect obtained by blending the component (D) is slightly insufficient.
- the concentration of the component (D) exceeds 5% by mass, the effect obtained by blending the component (D) is not improved so much.
- the surface treatment liquid further contains (E) phosphoric acid (hereinafter, also referred to as “(E) component”).
- (E) component phosphoric acid
- the concentration of the component (E) in the surface treatment liquid is preferably 0.05 to 5% by mass, more preferably 0.1 to 4% by mass, and 0.3 to 2% by mass. Is particularly preferable.
- concentration of the component (E) is less than 0.05% by mass, the effect obtained by blending the component (E) is slightly insufficient.
- the concentration of the component (E) exceeds 5% by mass, the effect obtained by blending the component (E) is not improved so much.
- the surface treatment liquid is an aqueous solution in which each component is dissolved in water. Therefore, the surface treatment liquid contains water as a solvent.
- the amount of water in the surface treatment liquid is preferably the balance depending on the concentrations of the above-mentioned components (A) to (E).
- the content of water in the surface treatment liquid is preferably the balance depending on the concentrations of the components (A) to (E) and the additives.
- the content of water in the surface treatment liquid may be about 60 to 99% by mass.
- the surface treatment liquid may further contain well-known additives as long as the effects of the present invention are not impaired.
- additives stabilizers, solubilizers for each component, defoaming agents, pH adjusters, specific gravity adjusters, viscosity adjusters, wettability improvers, chelating agents, oxidizing agents, reducing agents, and surfactants. Etc. can be mentioned.
- concentrations of these additives are generally in the range of 0.001 to 10% by mass, respectively.
- a surface treatment method for a nickel-containing material which is an embodiment of the present invention has a step of bringing the surface treatment solution described above into contact with the surface of the nickel-containing material.
- the method of bringing the surface treatment liquid into contact with the surface of the nickel-containing material is not particularly limited, and a general pretreatment method can be adopted.
- the surface treatment liquid can be brought into contact with the surface of the nickel-containing material by a pretreatment method such as a dip method, a spray method, or a spin method.
- the nickel-containing material When the surface of the nickel-containing material is surface-treated by the dip method, for example, the nickel-containing material may be immersed in the surface treatment solution adjusted to a temperature range of 10 to 90 ° C. for about 1 to 600 seconds.
- a surface treatment liquid adjusted to a temperature range of 10 to 90 ° C. is applied to the surface of the nickel-containing material at a pressure of 0.01 to 1.0 MPa. Just spray it.
- the surface treatment liquid is contacted with the surface of the nickel-containing material for treatment, it is washed with pure water and dried.
- a resist pattern is formed on the surface of the nickel-containing material by a conventionally known method, and then etching is performed with an etching solution, whereby fine wiring having good adhesion to the resist pattern can be formed.
- the above-mentioned surface treatment liquid and the surface treatment method using this surface treatment liquid process for example, a nickel-containing material for electrodes and wiring of devices such as liquid crystal displays, plasma displays, touch panels, organic ELs, solar cells, and lighting equipment. It can be used suitably when
- A-1 Iron (III) sulfate
- A-2 Iron (III) chloride
- B-1 Sulfuric acid
- B-2 Hydrochloric acid
- C-1 triammonium citrate
- C-2 ammonium lactate
- C-3 ammonium formate
- C-4 diammonium hydrogen citrate
- C-5 ammonium tartrate
- C-6 ammonium sulfate
- C-7 citric acid
- E-1 Phosphoric acid
- Example 1 ⁇ Nickel-containing material surface treatment liquid> (Example 1 and Comparative Example 1)
- the respective components were mixed so as to have the composition shown in Table 1, and treated liquid No. 1 to 17 were obtained.
- the concentration of component (A) represents the concentration of ferric ion
- the concentration of component (B) represents the concentration of sulfuric acid or hydrogen chloride. Water was added so that the total of the components would be 100% by mass.
- Example 2-1 An Fe—Ni 36% foil (hereinafter, also referred to as “(untreated) substrate”) having a length of 100 mm ⁇ a width of 100 mm ⁇ a thickness of 0.030 mm was prepared.
- the treatment liquid No. was applied to this surface under the conditions of 35 ° C. and a spray pressure of 0.1 MPa. 1 was sprayed by a spray method, and then sequentially washed with 3 mass% hydrochloric acid and ion-exchanged water.
- a ferric chloride-based pattern etching solution (trade name “Adeka Kermica IN-654”, manufactured by ADEKA) under a spray pressure of 0.1 MPa was sprayed (50 ° C., 150 seconds) by a spray method for etching.
- the substrate was washed with 3% by mass hydrochloric acid and ion-exchanged water in order, and the substrate No. Got 1.
- Example 2-2 to 2-10 Treatment liquid No. Instead of the treatment liquid No. Example substrate No. 2 was used in the same manner as in Example 2-1 except that Nos. 2 to 10 were used. 2-10 were obtained.
- Maximum thickness of smut is less than 10 nm ++: Maximum thickness of smut is 10 nm or more and less than 30 nm +: Maximum thickness of smut is 30 nm or more and less than 50 nm-: Maximum thickness of smut is 50 nm or more and less than 100 nm ---: Maximum thickness of smut is 100 nm or more and less than 300 nm ---: The maximum smut thickness is 300 nm or more
- the example substrate No From the results shown in Table 2, the example substrate No. It can be seen that in Examples 1 to 10, the formation of smut is sufficiently suppressed and the adhesiveness of the resist pattern is good, as compared with Comparative Examples 1 to 8. Further, comparing the results of Evaluation Examples 1-1 to 1-7 with the results of Evaluation Examples 1-8 to 1-9, ferric sulfate was used as the component (A) and sulfuric acid was used as the component (B). It can be seen that the adhesiveness of the resist pattern is particularly good when used. Furthermore, by comparing the results of Evaluation Examples 1-1 to 1-9 with the results of Evaluation Example 1-10, it can be seen that good results are obtained when the treatment liquid containing formic acid or phosphoric acid is used.
- the surface treatment liquid for a nickel-containing material capable of suppressing the formation of smut when etching the nickel-containing material and improving the adhesion between the resist pattern and the nickel-containing material.
- the surface treatment method of a nickel containing material can be provided.
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Abstract
Description
(A)成分として、以下に示すA-1及びA-2を用意した。
A-1:硫酸鉄(III)
A-2:塩化鉄(III)
(B)成分として、以下に示すB-1及びB-2を用意した。
B-1:硫酸
B-2:塩酸
(C)成分として、以下に示すC-1~C-7を用意した。
C-1:クエン酸三アンモニウム
C-2:乳酸アンモニウム
C-3:ギ酸アンモニウム
C-4:クエン酸水素二アンモニウム
C-5:酒石酸アンモニウム
C-6:硫酸アンモニウム
C-7:クエン酸
(D)成分として、以下に示すD-1を用意した。
D-1:ギ酸
(E)成分として、以下に示すE-1を用意した。
E-1:リン酸
(実施例1及び比較例1)
表1に示す配合となるように各成分を混合して、処理液No.1~17を得た。表1中、(A)成分の濃度は第二鉄イオンの濃度を表しており、(B)成分の濃度は硫酸又は塩化水素の濃度を表している。なお、成分の合計が100質量%となるように水を配合した。
(実施例2-1)
縦100mm×横100mm×厚さ0.030mmのFe-Ni36%箔(以下、「(未処理の)基体」とも記す)を用意した。この表面に35℃、スプレー圧0.1MPaの条件で処理液No.1をスプレー法により噴霧した後、3質量%塩酸及びイオン交換水で順次洗浄した。ドライフィルムレジストを用いて、基体上にライン/スペース=10μm/10μmのレジストパターンを30箇所形成した。次いで、スプレー圧0.1MPaの条件で塩化第二鉄系パターンエッチング液(商品名「アデカケルミカIN-654」、ADEKA社製)をスプレー法により噴霧(50℃、150秒)してエッチングした後、3質量%塩酸及びイオン交換水で順次洗浄し、実施例基体No.1を得た。
処理液No.1に代えて、処理液No.2~10をそれぞれ用いたこと以外は、前述の実施例2-1と同様にして実施例基体No.2~10を得た。
処理液No.1に代えて、処理液No.11~17をそれぞれ用いたこと以外は、前述の実施例2-1と同様にして比較例基体1~7を得た。
ドライフィルムレジストを用いて、未処理の基体上にライン/スペース=10μm/10μmのレジストパターンを30箇所形成した。次いで、スプレー圧0.1MPaの条件で塩化第二鉄系パターンエッチング液(商品名「アデカケルミカIN-654」、ADEKA社製)をスプレー法により噴霧(50℃、150秒)してエッチングした後、3質量%塩酸及びイオン交換水で順次洗浄し、比較例基体8を得た。また、未処理の基体を比較例基体9とした。
(スマット評価)
X線光電子分光分析装置を使用し、実施例基体No.1~10及び比較例基体1~9の表面に析出しているスマットの最大厚みを測定し、以下に示す評価基準にしたがって評価した。結果を表2に示す。
+++:スマットの最大厚みが10nm未満
++:スマットの最大厚みが10nm以上30nm未満
+:スマットの最大厚みが30nm以上50nm未満
-:スマットの最大厚みが50nm以上100nm未満
--:スマットの最大厚みが100nm以上300nm未満
---:スマットの最大厚みが300nm以上
基体を観察し、以下に示す評価基準にしたがってレジストパターンの密着性を評価した。結果を表2に示す。
+++:30箇所全てのレジストパターンが基体上に保持されていた。
++:28~29箇所のレジストパターンが基体上に保持されていた。
+:26~27箇所のレジストパターンが基体上に保持されていた。
--:24~25箇所のレジストパターンが基体上に保持されていた。
---:20~23箇所のレジストパターンが基体上に保持されていた。
----:19以下の箇所のレジストパターンが基体上に保持されていた。
Claims (4)
- ニッケル含有材料の表面を処理するための表面処理液であって、
(A)第二鉄イオン0.05~5質量%;
(B)無機酸0.5~20質量%;
(C)クエン酸三アンモニウム、乳酸アンモニウム、ギ酸アンモニウム、クエン酸水素二アンモニウム、グリコール酸アンモニウム、及びリンゴ酸アンモニウムからなる群より選択される少なくとも1種の化合物1~20質量%;及び
水を含有する水溶液である表面処理液。 - さらに、(D)ギ酸0.05~5質量%を含有する請求項1に記載の表面処理液。
- さらに、(E)リン酸0.05~5質量%を含有する請求項1又は2に記載の表面処理液。
- 請求項1~3のいずれか一項に記載の表面処理液をニッケル含有材料の表面に接触させる工程を有するニッケル含有材料の表面処理方法。
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JP2020552935A JPWO2020079977A1 (ja) | 2018-10-17 | 2019-09-04 | 表面処理液及びニッケル含有材料の表面処理方法 |
KR1020217014245A KR20210075151A (ko) | 2018-10-17 | 2019-09-04 | 표면 처리액 및 니켈 함유 재료의 표면 처리 방법 |
CN201980068276.4A CN112867811A (zh) | 2018-10-17 | 2019-09-04 | 表面处理液和含镍材料的表面处理方法 |
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- 2019-09-04 JP JP2020552935A patent/JPWO2020079977A1/ja active Pending
- 2019-09-04 KR KR1020217014245A patent/KR20210075151A/ko active Search and Examination
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JPH04228599A (ja) * | 1990-04-30 | 1992-08-18 | Atochem North America Inc | 3価クロム浴を再生するための装置及び方法 |
JP2009235456A (ja) * | 2008-03-26 | 2009-10-15 | Okuno Chem Ind Co Ltd | 3価クロムめっき皮膜用電解処理液 |
JP2016025358A (ja) * | 2014-07-24 | 2016-02-08 | エア プロダクツ アンド ケミカルズ インコーポレイテッドAir Products And Chemicals Incorporated | 窒化チタンハードマスク及びエッチ残留物除去 |
JP2016060918A (ja) * | 2014-09-16 | 2016-04-25 | 株式会社Jcu | 装飾用3価クロムめっき液およびこれを利用した装飾クロムめっき方法 |
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