CN104894569B - Ni-Pd metal surface treatment agent - Google Patents
Ni-Pd metal surface treatment agent Download PDFInfo
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- CN104894569B CN104894569B CN201510375623.1A CN201510375623A CN104894569B CN 104894569 B CN104894569 B CN 104894569B CN 201510375623 A CN201510375623 A CN 201510375623A CN 104894569 B CN104894569 B CN 104894569B
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 34
- 239000002184 metal Substances 0.000 title claims abstract description 34
- 239000012756 surface treatment agent Substances 0.000 title description 2
- -1 phosphoric acid compound Chemical class 0.000 claims abstract description 22
- 239000002262 Schiff base Substances 0.000 claims abstract description 21
- 238000005260 corrosion Methods 0.000 claims abstract description 14
- 230000007797 corrosion Effects 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 150000002391 heterocyclic compounds Chemical class 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims description 11
- 150000004753 Schiff bases Chemical class 0.000 claims description 6
- 239000005416 organic matter Substances 0.000 claims description 6
- 125000005499 phosphonyl group Chemical group 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 5
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- JWYUFVNJZUSCSM-UHFFFAOYSA-N 2-aminobenzimidazole Chemical class C1=CC=C2NC(N)=NC2=C1 JWYUFVNJZUSCSM-UHFFFAOYSA-N 0.000 claims description 3
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical class OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 3
- 229940120146 EDTMP Drugs 0.000 claims description 2
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 2
- 241001272567 Hominoidea Species 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 claims description 2
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 claims description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N aminothiocarboxamide Natural products NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 229940116269 uric acid Drugs 0.000 claims description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims 2
- 150000001412 amines Chemical class 0.000 claims 1
- 150000003009 phosphonic acids Chemical class 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 2
- 239000003112 inhibitor Substances 0.000 abstract 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 17
- 229910052759 nickel Inorganic materials 0.000 description 9
- 230000003750 conditioning effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 229910052763 palladium Inorganic materials 0.000 description 5
- 238000003466 welding Methods 0.000 description 5
- 239000004480 active ingredient Substances 0.000 description 4
- 239000007769 metal material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 210000000981 epithelium Anatomy 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 206010028980 Neoplasm Diseases 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 244000247747 Coptis groenlandica Species 0.000 description 1
- 235000002991 Coptis groenlandica Nutrition 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 229910002666 PdCl2 Inorganic materials 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Landscapes
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention provides a Ni-Pd metal surface treating agent which is high-temperature resistant and corrosion resistant and has good weldability after Ni-Pd metal is treated. The Ni-Pd metal surface treating agent is characterized by mainly comprising a corrosion inhibitor and a surfactant, wherein the effective components of the corrosion inhibitor are the compound of an organic phosphoric acid compound, a Schiff base compound and an N, S heterocyclic compound, the surfactant mainly adopts one or more nonionic surfactants, and the pH value of the Ni-Pd metal surface treating agent is controlled to be below 10.
Description
Technical field
The present invention relates to Ni-Pd metal conditioners.
Technical background
Nickel coating, palladium coating by its a variety of excellent chemistry and mechanical properties have been used for aviation, automobile, electric mechanical,
The multiple fields such as petrochemical industry, electroless plating Ni-Au, electroless plating Ni-Pd-Au are used for the electronic units such as substrate, lead frame.Using
Electroless form obtains nickel dam, obtains a Ceng Ba islands by the method for chemistry displacement palladium on nickel coating surface, passes through the technique
Still there is part of nickel exposed metal/bare metal obtained Ni-Pb metal surfaces in air.Ni, Pd are easily oxidized by the air at high temperature, shadow
Its weldability energy is rung, so needing to form one layer of protection epithelium on its surface using other corrosion inhibiter.
Existing technology is handled for single metallic surface more, and is not suitable with alloy or more Treatment of Metal Surface, and very
Difficulty makes metal material while has anti-oxidant, corrosion-resistant and excellent welding performance, and Patents documents have CN
201180010000 and CN201110075074, there is problem above.
The content of the invention
It is an object of the present invention to provide a kind of surface conditioning agent used for Ni-Pd metals, by surface conditioning agent
Active ingredient Ni-Pd metal surfaces formed organic coating, make it have anti-oxidant, corrosion-resistant and excellent welding performance,
So that Ni-Pd metals are advantageous to the preparation of the electronic units such as substrate, lead frame.
A kind of Ni-Pd metal conditioners, are mainly made up of corrosion inhibiter and surfactant；
The corrosion inhibiter, mainly by organophosphor acid compounds, Schiff bases compound, N, S heterocyclic compound and halogen
Element or halide salts compound to obtain；
Organophosphor acid compounds are the organic matter or its salt that intramolecular contains phosphonyl group, contain the organic of phosphonyl group
Thing is ethylenediamine tetramethylene phosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, diethylene triamine pentamethylene phosphonic, the methene phosphine of diethylenetriamine five
Acid or ATMP；Organic matter salt containing phosphonyl group is alkali metal salt (particular certain cancers, sylvite)；Organic phosphoric acid
The molar ratio 50~100: 5~25: 1~5 that class compound, Schiff bases compound are compounded with N, S heterocyclic compound；
Schiff bases compound has contracting sulfamido schiff bases, contracting amino acids schiff bases, contracting Thiourea schiff bases, contracting acid amides
Class schiff bases etc., wherein it is preferred that contracting amino acids schiff bases；
N, S heterocyclic compounds are 2- aminobenzimidazoles, BTA, 2-mercaptobenzothiazole or uric acid.
Using the organophosphor acid compounds of one or more, one or more kinds of Schiff bases compounds and one
Kind or more than one N, S heterocyclic compound compounded, in three kinds of compositions the control of every kind of Ingredient Amount 0.001~
500mmol/L, preferably 0.01~100mmol/L.
The present invention can use one or more kinds of nonionic surfactants, preferably APES type,
High-carbon fatty alcohol polyoxyethylene ether type and fatty acid methyl ester ethoxylate type.The above-mentioned total dosage control of surfactant is 0.01
~100mmol/L, more preferably 0.1~50mmol/L.
Described halogen or halide salts, metallic surface passivating film is dissolved by active anion, so as to form new guarantor
Cuticula, its salt are mainly alkali metal salt, particular certain cancers, sylvite.
The Ni-Pd metal conditioners of the material composition, it is characterised in that the pH controls of surface conditioning agent 1~
10, preferably 1~7.
A kind of Ni-Pd metals, nickel dam is obtained using electroless form, and palladium is replaced by chemistry on nickel coating surface
Method obtain a Ceng Ba islands, part of nickel exposed metal/bare metal is left in air in the Ni-Pd metal surfaces obtained by the technique.
When the surface conditioning agent using the present invention is surface-treated to metal, epithelium is formed using dipping or spraying
Method, preferably infusion process.Shape for metal to be treated can be any shape such as wire, plate, band, granular, by using
The surface conditioning agent of the present invention, after being surface-treated to Ni-Pd metal surfaces, it can be made to obtain excellent in oxidation resistance, weldering
The characteristics of expecting wetability.
Corrosion inhibiter main component organophosphor acid compounds of the present invention, Schiff bases compound and N, S are miscellaneous
The metallic atom of cycle compound energy metal material surface is attracted to metal material table by different degrees of coordination
Face, at the same the types of functionality group that carries of such compound by mutual synergistic function can metal material surface formed with
Machine epithelium and play corrosion inhibition.For the present invention by testing after 155 DEG C are incubated 20 hours, its welding performance keeps good.
Specific embodiment
Embodiment 1~6；Comparative example 1~8
13 kinds of surface conditioning agents are configured, after being incubated 20 hours at 155 DEG C after its active ingredient and film forming, bonding test result
Such as table 1.
Ni-Pd metal surfaces are obtained on substrate to obtain by the following method.
Alkali cleaning oil removing (10%NaOH, 2 minutes) → washing (normal temperature, 1 minute) → pickling (10%H2SO4, 1 minute) → water
Washing (normal temperature, 1 minute) → microetch (potassium peroxydisulfate 0.37mol/L, sulfuric acid 20ml, 3 minutes), → washing (normal temperature, 1 minute) → is living
Change (YC-42,3 minutes) → washing (normal temperature, 1 minute) → chemical nickel plating (YC-51M 100mL/L, YC-51A 48mL/L, YC-
51D 4mL/L, 84 DEG C, 8 minutes) → washing (normal temperature, 1 minute) → chemical palladium immersing (PdCl29mmol/L, ammoniacal liquor 80ml/L, lemon
Lemon acid 26mmol/L, OP-100.01ml/L, 40 DEG C, 30 minutes) → washing (normal temperature, 1 minute) → drying
The configuration of surface conditioning agent：
Corresponding surfactant is weighed by formula to be dissolved in distilled water, stirring is abundant to dissolving, and is dissolving sufficient table
Added in existing activator solution and be formulated the desired amount of all kinds of corrosion inhibiter materials, stirring is abundant to dissolving, and adjusts pH, static 30min
Constant volume afterwards.
Obtained metal is impregnated 0.5~15 minute in the surface conditioning agent configured at 0~100 DEG C, preferably 25~
Impregnated 1.5~10 minutes at 50 DEG C.
To 10, the film forming sample of each embodiment, after being handled 20 hours at 155 DEG C, bonding test is carried out, bonding is surveyed
The resistance to elevated temperatures and the welding performance after high-temperature process of the direct reacting metal of test result.
Bonding equipment:Hughes 2460II
Test equipment:Dages Series 4000
Beat gold thread：K&S Mod.4129,
Bonding pressure:5cN
Bonding time:5sec
Pulling force about 30cN
The different surface treatment agent of table 1,20 hours bonding test results are incubated at 155 DEG C after its active ingredient and film forming
By table above it can be seen that not reaching required effect as corrosion inhibiter active ingredient using schiff bases, work as schiff bases
With significant effect can be obtained when ATMP, 2- aminobenzimidazole collective effects, when Schiff alkali concn increases
Pull-off force increases, while the proportioning of each component can reach excellent effect in preferred scope, otherwise DeGrain；Adopt
The effect using nonionic Surfactant can not be reached with the effect of anionic surfactant sodium dodecylbenzene sulfonate；Make
It is more notable than using stearic acid welding effect with N, S heterocyclic compound；Metal after processed by the invention compared to comparative example 6
Effect is more excellent.
Claims (5)
1. a kind of Ni-Pd metal conditioners, it is characterised in that be mainly made up of corrosion inhibiter and nonionic surfactant；Institute
Corrosion inhibiter is stated, is answered by organophosphor acid compounds, Schiff bases compound and N, S heterocyclic compound and halogen or halide salts
With obtaining；Described organophosphor acid compounds are the organic matter or its salt that intramolecular contains phosphonyl group, wherein containing phosphonic acids
The organic matter of group is ethylenediamine tetramethylene phosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, diethylene triamine pentamethylene phosphonic, divinyl three
One or more in the methylenephosphonic acid of amine five, ATMP；Organic matter salt containing phosphonyl group contains to be described
There are the one or more in the organic matter alkali metal salt of phosphonyl group；
Described Schiff bases compound is contracting sulfamido schiff bases, contracting amino acids schiff bases, contracting Thiourea schiff bases or contracting
Amide-type schiff bases；
N, S heterocyclic compounds are 2- aminobenzimidazoles, BTA, 2-mercaptobenzothiazole or uric acid；
The molar ratio 50~100: 5 that organophosphor acid compounds, Schiff bases compound are compounded with N, S heterocyclic compound
~25: 1~5；
In three kinds of organophosphor acid compounds, Schiff bases compound and N, S heterocyclic compound compositions, the dosage of every kind of composition is equal
Control is in 0.001~500mmol/L.
2. Ni-Pd metal conditioners as claimed in claim 1, it is characterised in that described nonionic surfactant
For APES, high-carbon fatty alcohol polyoxyethylene ether or fatty acid methyl ester ethoxylate.
3. Ni-Pd metal surfactants as claimed in claim 1 or 2, it is characterised in that using one or more kinds of
Nonionic surface active agent, its total dosage control is in 0.01~100mmol/L.
4. Ni-Pd metal surfactants as claimed in claim 1 or 2, it is characterised in that described metal conditioner
PH control 1~10.
5. Ni-Pd metal surfactants as claimed in claim 4, it is characterised in that described metal conditioner
PH is controlled 1~7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510375623.1A CN104894569B (en) | 2015-06-30 | 2015-06-30 | Ni-Pd metal surface treatment agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510375623.1A CN104894569B (en) | 2015-06-30 | 2015-06-30 | Ni-Pd metal surface treatment agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104894569A CN104894569A (en) | 2015-09-09 |
| CN104894569B true CN104894569B (en) | 2018-03-02 |
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|---|---|---|---|
| CN201510375623.1A Expired - Fee Related CN104894569B (en) | 2015-06-30 | 2015-06-30 | Ni-Pd metal surface treatment agent |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424435A (en) * | 2002-12-20 | 2003-06-18 | 上海电力学院 | Composite corrosion inhibitor containg mercapto-heterocyclic compound and alkali metal iodide |
| JP4518507B2 (en) * | 2004-03-05 | 2010-08-04 | 日鉱金属株式会社 | Metal surface treatment agent |
| CN102782189A (en) * | 2010-12-01 | 2012-11-14 | 吉坤日矿日石金属株式会社 | Surface treatment agent for pd or alloy mainly composed of pd, and surface coating layer structure of copper surface |
| CN103849879A (en) * | 2014-03-26 | 2014-06-11 | 西安石油大学 | Gemini type bimolecular Sciff base waste water corrosion inhibitor and preparation method thereof |
-
2015
- 2015-06-30 CN CN201510375623.1A patent/CN104894569B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424435A (en) * | 2002-12-20 | 2003-06-18 | 上海电力学院 | Composite corrosion inhibitor containg mercapto-heterocyclic compound and alkali metal iodide |
| JP4518507B2 (en) * | 2004-03-05 | 2010-08-04 | 日鉱金属株式会社 | Metal surface treatment agent |
| CN102782189A (en) * | 2010-12-01 | 2012-11-14 | 吉坤日矿日石金属株式会社 | Surface treatment agent for pd or alloy mainly composed of pd, and surface coating layer structure of copper surface |
| CN103849879A (en) * | 2014-03-26 | 2014-06-11 | 西安石油大学 | Gemini type bimolecular Sciff base waste water corrosion inhibitor and preparation method thereof |
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