CN100580154C - Release agent for electrolytic silver - Google Patents
Release agent for electrolytic silver Download PDFInfo
- Publication number
- CN100580154C CN100580154C CN200480007071A CN200480007071A CN100580154C CN 100580154 C CN100580154 C CN 100580154C CN 200480007071 A CN200480007071 A CN 200480007071A CN 200480007071 A CN200480007071 A CN 200480007071A CN 100580154 C CN100580154 C CN 100580154C
- Authority
- CN
- China
- Prior art keywords
- silver
- salt
- release agent
- electrolytic
- agent
- 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.)
- Expired - Lifetime
Links
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 48
- 239000004332 silver Substances 0.000 title claims abstract description 48
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 31
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 47
- 150000003839 salts Chemical class 0.000 claims abstract description 20
- -1 hydantoin compound Chemical class 0.000 claims abstract description 17
- 229940091173 hydantoin Drugs 0.000 claims abstract description 15
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims abstract description 13
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims abstract description 9
- 235000003704 aspartic acid Nutrition 0.000 claims abstract description 5
- CKLJMWTZIZZHCS-REOHCLBHSA-N aspartic acid group Chemical group N[C@@H](CC(=O)O)C(=O)O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims abstract description 5
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 claims abstract description 5
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical group O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 claims abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 238000002845 discoloration Methods 0.000 claims description 4
- 229960002989 glutamic acid Drugs 0.000 claims description 4
- 239000006174 pH buffer Substances 0.000 claims description 4
- POJWUDADGALRAB-UHFFFAOYSA-N allantoin Chemical compound NC(=O)NC1NC(=O)NC1=O POJWUDADGALRAB-UHFFFAOYSA-N 0.000 abstract 2
- IVQCQIORBPXQGP-UHFFFAOYSA-N 3-(hydroxymethyl)-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)NC(=O)N(CO)C1=O IVQCQIORBPXQGP-UHFFFAOYSA-N 0.000 abstract 1
- YIROYDNZEPTFOL-UHFFFAOYSA-N 5,5-Dimethylhydantoin Chemical compound CC1(C)NC(=O)NC1=O YIROYDNZEPTFOL-UHFFFAOYSA-N 0.000 abstract 1
- POJWUDADGALRAB-PVQJCKRUSA-N Allantoin Natural products NC(=O)N[C@@H]1NC(=O)NC1=O POJWUDADGALRAB-PVQJCKRUSA-N 0.000 abstract 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 abstract 1
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 abstract 1
- 229960000458 allantoin Drugs 0.000 abstract 1
- 235000013922 glutamic acid Nutrition 0.000 abstract 1
- 239000004220 glutamic acid Substances 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 230000003746 surface roughness Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 7
- 239000010408 film Substances 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000003287 bathing Methods 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 2
- PSLCKQYQNVNTQI-BHFSHLQUSA-N (2s)-2-aminobutanedioic acid;(2s)-2-aminopentanedioic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O.OC(=O)[C@@H](N)CCC(O)=O PSLCKQYQNVNTQI-BHFSHLQUSA-N 0.000 description 1
- ODHCTXKNWHHXJC-UHFFFAOYSA-N 5-oxoproline Chemical compound OC(=O)C1CCC(=O)N1 ODHCTXKNWHHXJC-UHFFFAOYSA-N 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical class N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 238000003909 pattern recognition Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229960002317 succinimide Drugs 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F5/00—Electrolytic stripping of metallic layers or coatings
Abstract
A release agent for electrolytic silver. The release agent contains no cyanide, has a long life, and is highly effective in silver release from edge sides. It inhibits the necessary silver surface parts from having unevenness of surface roughness or an increased gloss after silver release. The release agent for electrolytic silver comprises a hydantoin compound and an aminocarboxylic acid or salt thereof as major ingredients. The hydantoin compound preferably is hydantoin, 5,5-dimethylhydantoin, 5,5-dimethyl-3-hydroxymethylhydantoin, allantoin, or a salt of any of these. The aminocarboxylic acid or salt preferably is aspartic acid, glutamic acid, or a salt of either.
Description
Technical field
The present invention relates to the release agent for electrolytic of silver, particularly the release agent for electrolytic of the silver of the unwanted part of the suitable silver-plated film of electrolytic stripping.
Background technology
As non-cyanogen class silver stripper, that has filed an application has, succinimide or phthalic imidine (for example opening flat 2-104699 communique) with reference to the spy, have-5,6 membered ring compounds (for example opening flat 2-175825 communique) of NH-with reference to the spy, 2-Pyrrolidone-5-carboxylic acid (for example opening flat 6-41800 communique), hydantoin compound (for example opening flat 7-243100 communique) etc. with reference to the spy with reference to the spy, but former three is because of the decomposition fierceness of bathing, so there is the problem that consumption is many, bathe the life-span weak point.On the other hand, then there is the problem that is easy to generate injustice, glossiness rising on the silver-colored face that needs part in hydantoin compound because the bath decomposition of little so consumption is few, the life-span is long, is peeled off if still carry out silver in order to boost productivity with high current density.
In order to address this problem, open in flat 9-49100 number (No. the 2939181st, Japanese Patent) communique the spy and to disclose, by be main component with hydantoin compound, tricyanic acid etc., to wherein adding boron compound as submember, can realize that long and silver-colored face that obtain with high current density of life-span does not have injustice.
Summary of the invention
But, when silver-colored stripper being used for lead frame etc., as nearest needs, the requirement raising is leaked at the stripping ability that does not need silver partly on the side of lead frame and is suppressed the rising that silver-colored stripper is handled the glossiness of necessity silver-colored face partly after not needing part gradually.Along with the miniaturization of lead frame, leak the reason that is known as migration at lateral silver.In addition, we can say,, then can bring detrimentally affect the pattern recognition of wire bonds (wire bond) if glossiness is too high.
The invention provides the release agent for electrolytic silver that satisfies these needs, the object of the present invention is to provide a kind of release agent for electrolytic silver, the generation of the injustice of the silver-colored face of the necessary part that it is a non-cyano group class silver stripper, the life-span is long, the side stripping ability is strong and can suppress silver after peeling off and the rising of glossiness.
Present inventors found that by following formation release agent for electrolytic silver through further investigation, can solve above-mentioned problem.That is, the present invention is as follows.
(1) a kind of release agent for electrolytic silver is a main component with hydantoin compound and aminocarboxylic acid or its salt.
(2) as above-mentioned (1) described release agent for electrolytic silver, described aminocarboxylic acid is the mono amino dicarboxylic acid.
(3) as above-mentioned (1) or (2) described release agent for electrolytic silver, as described hydantoin compound, with glycolylurea, 5,5-T10,5,5-T10-3-methylol, wallantoin or their salt are main component, as described aminocarboxylic acid or its salt, be main component with aspartic acid, L-glutamic acid or their salt.
Silver-colored electrolytic stripping liquid of the present invention is a main component with hydantoin compound and aminocarboxylic acid or its salt.The present application people finds, by using hydantoin compound, can prolonging the life-span of bath, and then by using aminocarboxylic acid or its salt, can improve the silver plated stripping ability that does not need part, and the glossiness that can suppress to peel off the silvered face that does not need the necessary part behind part silver-plated rises and uneven generation.
Embodiment
Hydantoin compound as one of main component of release agent for electrolytic silver of the present invention preferably uses the glycolylurea shown in the following chemical formula, 5,5-T10,5,5-T10-3-methylol, wallantoin or their salt.As salt, particular certain cancers, sylvite etc.
Glycolylurea 5, the 5-T10
5,5-T10-3-methylol wallantoin
The concentration range of these materials in bath is 1～500g/L, is preferably 5～200g/L.If concentration is low excessively, then be easy to generate the passivation of silver, on the other hand, and if the problem that stripper (stripping liquid) oozes out then appears in excessive concentration, thus not preferred.
As the aminocarboxylic acid of one of release agent for electrolytic silver main component of the present invention, preferred mono amino dicarboxylic acid, preferred especially aspartic acid, L-glutamic acid or their salt.The chemical formula of aspartic acid and L-glutamic acid is shown below.As salt, particular certain cancers, sylvite.
Aspartic acid L-glutamic acid
The concentration range of these materials in bath is 1～500g/L, is preferably 5～200g/L.If concentration is low excessively, side stripping ability and to suppress the injustice of the silver-colored face of necessary part, effect that glossiness rises low, on the other hand then, if excessive concentration, then effect is saturated, thereby not preferred.
And then can also be as required, in release agent for electrolytic silver of the present invention, add pH buffer reagent, tensio-active agent, copper discoloration and prevent that agent, epoxy are anti-and ooze out agent etc.These pH buffer reagents, tensio-active agent, copper discoloration prevent that agent, epoxy are anti-and ooze out agent etc. and can use known material.
Use above-mentioned stripper, under defined terms, carry out the electrolytic stripping of silver.Adjust agent with alkali metal hydroxide such as sodium hydroxide or the such pH of alkaline-earth metal oxyhydroxide and adjust stripper, make pH become 7 or it is above, preferably become 9～12.If pH is low excessively, then slow, the lift-off processing of peeling rate does not need the silver-colored face of the necessary part after the part easily to produce injustice, selects separability poor.On the other hand, even pH is too high, there is not advantage yet.
In addition, in the present invention, as object being treated, on the various metal base material of the such iron nickel alloy of copper, copper alloy, 42 alloys, stainless steel, nickelalloy etc., to have formed the material of silver-colored tunicle as peeling off object by silver-plated, weldering silver etc.
The object being treated of such tunicle that is formed with silver on the surface is immersed in the bath of the above-mentioned release agent for electrolytic that adjusts like that, is that anode carries out electrolysis with this object being treated.Anticathode material has no particular limits, and generally uses stainless steel.Current density is taken as 0.1～50A/dm with respect to the area of the silver of peeling off
2, preferably be taken as 0.5～20A/dm
2If current density is low excessively, then peeling rate is slow, on the other hand, if current density is too high, then because cause the passivation of silver thereby not preferred easily.In addition, it is 5 ℃ or more than it, preferably carry out electrolysis bathing temperature at 10～60 ℃.Temperature low with excessivelying, then peeling rate is slow if bathe, on the other hand, if so too high, then be not suitable for because bathe the instability that becomes.In addition, the stirring of preferably in electrolytic process, bathing, particularly under the high situation of current density, in order not cause passivation, preferred fast stirring velocity.
When utilizing stripper to bathe to peel off the silver-plated film of part of object being treated, can adopt, cover the silver-plated film of the necessary part that should not peel off, method that only dipping should released part partly.In addition, fully thick at the silver-plated film of necessity part, can with not needing of should peeling off situation that part peels off with same degree ground under, also can flood whole.In addition, when being object being treated with the lead frame, because the silver-plated thickness of part such as the needs of pad, lead-in wire etc., the silver-plated thin film thickness that does not need part of lead-in wire side etc., even direct electrolytic stripping also can only be peeled off the silver-plated film that does not need part so do not cover the silver-plated part of necessary part.
Embodiment
Below, illustrate in greater detail the present invention by embodiment.
Embodiment 1～8, comparative example 1～3
The peel off bath of modulation as showing to form shown in 1-1, table 1-2 and the table 1-3.As sample, the lead frame of SOP class of 28 pins (pin) of silver point plating of copper strike plating, the 5 μ m of 0.05 μ m has been carried out in use all sidedly on Cu alloy material, be immersed in above-mentioned peeling off in the bath, carry out electrolytic stripping with the stripping conditions shown in table 1-1, table 1-2 and the table 1-3.
To the sample after peeling off, carry out following evaluation.
Silver face outward appearance and base material face outward appearance
By range estimation and microscopic examination (* 50), observe uneven, defective.With what can't see gentle defective not serves as good.
Silver face glossiness
Utilize Grossmeters (big Japanese ス Network リ one Application, DM-400) to measure.The big more expression glossiness of numerical value is high more.Silver-colored face glossiness before silver is peeled off is 0.40.
The silver peeling rate
Utilize fluorescent X-ray film thickness gauge (Seiko electronic industry, SFT-3200), measure the silver-plated thickness that silver is peeled off front and back, calculate silver-colored peeling rate.
The side stripping ability
Utilize microscope (* 50) to observe lateral silver and peel off state.What be stripped from lateral silver serves as good.
Table 1-1, table 1-2 and table 1-3 illustrate evaluation result.
Table 1-1
Silver-colored face glossiness before silver is peeled off is 0.40 (the big more glossiness of numerical value is high more)
Table 1-2
Silver-colored face glossiness before silver is peeled off is 0.40 (the big more glossiness of numerical value is high more)
Table 1-3
Silver-colored face glossiness before silver is peeled off is 0.40 (the big more glossiness of numerical value is high more)
With hydantoin compound of the present invention and aminocarboxylic acid or its salt is the release agent for electrolytic silver of main component, long, side stripping ability height of life-span and also can suppress silver and peel off after the silver-colored face of necessary part produce not gentle glossiness and rise.
Claims (4)
1. release agent for electrolytic silver, by hydantoin compound and aminocarboxylic acid or its salt, and the pH buffer reagent, tensio-active agent, the copper discoloration that add as required prevent that agent, epoxy are anti-and ooze out agent and constitute.
2. release agent for electrolytic silver prevents by hydantoin compound, aminocarboxylic acid or its salt, pH buffer reagent, tensio-active agent, copper discoloration that agent, epoxy are anti-and oozes out agent and constitute.
3. release agent for electrolytic silver as claimed in claim 1 or 2, described aminocarboxylic acid are the mono amino dicarboxylic acid.
4. release agent for electrolytic silver as claimed in claim 1 or 2, described hydantoin compound is a glycolylurea, 5,5-T10,5,5-T10-3-methylol, wallantoin or their salt, described aminocarboxylic acid or its salt are aspartic acid, L-glutamic acid or their salt.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP082672/2003 | 2003-03-25 | ||
| JP2003082672 | 2003-03-25 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1761775A CN1761775A (en) | 2006-04-19 |
| CN100580154C true CN100580154C (en) | 2010-01-13 |
Family
ID=33094925
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200480007071A Expired - Lifetime CN100580154C (en) | 2003-03-25 | 2004-01-22 | Release agent for electrolytic silver |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JP4312201B2 (en) |
| KR (1) | KR20050108413A (en) |
| CN (1) | CN100580154C (en) |
| HK (1) | HK1087158A1 (en) |
| TW (1) | TWI247827B (en) |
| WO (1) | WO2004085716A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104404611B (en) * | 2014-11-28 | 2016-11-30 | 江门市瑞期精细化学工程有限公司 | A kind of release agent for electrolytic of copper alloy surface coating and preparation method thereof |
| TWI755229B (en) * | 2020-12-30 | 2022-02-11 | 力橋國際有限公司 | Silver-plated layer electrolytically-stripping agent without cyanide, and method for electrolytically stripping silver-plated layer |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2603800B2 (en) * | 1994-03-08 | 1997-04-23 | 日本エレクトロプレイテイング・エンジニヤース株式会社 | Silver electrolytic stripping solution and electrolytic stripping method using the same |
| JPH08337900A (en) * | 1995-06-08 | 1996-12-24 | N E Chemcat Corp | Electrolytically stripping agent for silver |
| JPH1088398A (en) * | 1996-09-11 | 1998-04-07 | Okuno Chem Ind Co Ltd | Electrolytic silver stripping agent, stripping solution and electrolytic stripping method |
| JP3225288B2 (en) * | 1997-10-07 | 2001-11-05 | 奥野製薬工業株式会社 | Silver electrolytic stripper |
-
2004
- 2004-01-22 JP JP2005503976A patent/JP4312201B2/en not_active Expired - Lifetime
- 2004-01-22 CN CN200480007071A patent/CN100580154C/en not_active Expired - Lifetime
- 2004-01-22 KR KR1020057017737A patent/KR20050108413A/en active Search and Examination
- 2004-01-22 WO PCT/JP2004/000534 patent/WO2004085716A1/en active Application Filing
- 2004-02-17 TW TW93103705A patent/TWI247827B/en not_active IP Right Cessation
-
2006
- 2006-06-28 HK HK06107314.8A patent/HK1087158A1/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| KR20050108413A (en) | 2005-11-16 |
| TW200424367A (en) | 2004-11-16 |
| CN1761775A (en) | 2006-04-19 |
| JP4312201B2 (en) | 2009-08-12 |
| HK1087158A1 (en) | 2006-10-06 |
| WO2004085716A1 (en) | 2004-10-07 |
| JPWO2004085716A1 (en) | 2006-06-29 |
| TWI247827B (en) | 2006-01-21 |
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Owner name: JX NIPPON MINING + METALS CORP. Free format text: FORMER OWNER: NIPPON MINING + METALS CO., LTD. Effective date: 20110324 |
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Address after: No.4, 10-fan, erdingmu, huzhimen, Tokyo, Japan Patentee after: JX NIPPON MINING & METALS Corp. Address before: Tokyo, Japan Patentee before: JX NIPPON MINING & METALS Corp. |
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