CN106222710A - A kind of acid half bright tin plating solution and preparation method thereof - Google Patents
A kind of acid half bright tin plating solution and preparation method thereof Download PDFInfo
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- CN106222710A CN106222710A CN201610742278.5A CN201610742278A CN106222710A CN 106222710 A CN106222710 A CN 106222710A CN 201610742278 A CN201610742278 A CN 201610742278A CN 106222710 A CN106222710 A CN 106222710A
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- 238000007747 plating Methods 0.000 title claims abstract description 48
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000002253 acid Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000001117 sulphuric acid Substances 0.000 claims abstract description 21
- 235000011149 sulphuric acid Nutrition 0.000 claims abstract description 21
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 15
- 239000001211 (E)-4-phenylbut-3-en-2-one Substances 0.000 claims abstract description 12
- 108010010803 Gelatin Proteins 0.000 claims abstract description 12
- 229940026189 antimony potassium tartrate Drugs 0.000 claims abstract description 12
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 12
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 12
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 12
- 229930008407 benzylideneacetone Natural products 0.000 claims abstract description 12
- WBTCZEPSIIFINA-MSFWTACDSA-J dipotassium;antimony(3+);(2r,3r)-2,3-dioxidobutanedioate;trihydrate Chemical compound O.O.O.[K+].[K+].[Sb+3].[Sb+3].[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O.[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O WBTCZEPSIIFINA-MSFWTACDSA-J 0.000 claims abstract description 12
- 229920000159 gelatin Polymers 0.000 claims abstract description 12
- 239000008273 gelatin Substances 0.000 claims abstract description 12
- 235000019322 gelatine Nutrition 0.000 claims abstract description 12
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 12
- 235000001968 nicotinic acid Nutrition 0.000 claims abstract description 12
- 229960003512 nicotinic acid Drugs 0.000 claims abstract description 12
- 239000011664 nicotinic acid Substances 0.000 claims abstract description 12
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims abstract description 12
- 235000010234 sodium benzoate Nutrition 0.000 claims abstract description 12
- 239000004299 sodium benzoate Substances 0.000 claims abstract description 12
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims abstract description 12
- BWHOZHOGCMHOBV-BQYQJAHWSA-N trans-benzylideneacetone Chemical compound CC(=O)\C=C\C1=CC=CC=C1 BWHOZHOGCMHOBV-BQYQJAHWSA-N 0.000 claims abstract description 12
- RFQOPUYDLCMQCE-UHFFFAOYSA-N 1-(2-hydroxyethyl)-5-nitropyrrole-2-carboxamide Chemical compound NC(=O)C1=CC=C([N+]([O-])=O)N1CCO RFQOPUYDLCMQCE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 8
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 8
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 30
- IVKNZCBNXPYYKL-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[4-(2,4,4-trimethylpentan-2-yl)phenoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO)C=C1 IVKNZCBNXPYYKL-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 229940014259 gelatin Drugs 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 claims description 2
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 abstract description 6
- 229950011260 betanaphthol Drugs 0.000 abstract description 3
- 230000000711 cancerogenic effect Effects 0.000 abstract description 3
- 231100000357 carcinogen Toxicity 0.000 abstract description 3
- 239000003183 carcinogenic agent Substances 0.000 abstract description 3
- 150000001299 aldehydes Chemical class 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 231100000614 poison Toxicity 0.000 abstract description 2
- 230000007096 poisonous effect Effects 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 description 16
- 238000000576 coating method Methods 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 14
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- -1 benzal Chemical class 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 229940044654 phenolsulfonic acid Drugs 0.000 description 2
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 description 1
- 150000004786 2-naphthols Chemical class 0.000 description 1
- BZOVBIIWPDQIHF-UHFFFAOYSA-N 3-hydroxy-2-methylbenzenesulfonic acid Chemical compound CC1=C(O)C=CC=C1S(O)(=O)=O BZOVBIIWPDQIHF-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000005451 methyl sulfates Chemical class 0.000 description 1
- 229950000081 metilsulfate Drugs 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
- C25D3/32—Electroplating: Baths therefor from solutions of tin characterised by the organic bath constituents used
Abstract
Invention describes a kind of acid half bright tin plating solution and preparation method thereof, belong to field of material surface treatment.Component and the content thereof of solution of the present invention are as follows: stannous sulfate 20 40g/L, sulphuric acid 80 110mL/L, benzylideneacetone 0.1 0.5g/L, OP 10 2 4mL/L, NP 10 1.5 3mL/L, sodium benzoate 0.9 1.5g/L, nicotinic acid 0.1 0.25g/L, gelatin 1 4g/L, ferrous sulfate 2 3g/L, ascorbic acid 0.5 1g/L, antimony potassium tartrate 0.5 1g/L, remaining is water.The solution dispersibility of the present invention and covering power are good, operating temperature range and cathode-current density wide ranges, and plating weldability is good, and adhesion is strong, and does not adds carcinogen Beta Naphthol 99MIN and poisonous aldehydes, and to human body and environmentally friendly, and cost reduces.
Description
Technical field
The present invention relates to a kind of acid half bright tin plating solution and preparation method thereof, belong to tin plating technical field.
Background technology
Acidic Sn electroplating is a kind of electroplating technology grown up the sixties.Tin plating to have toxicity low, good environmental protection, deposition
The advantages such as speed is fast, and current efficiency is high and corrosion resistance is good, the most gradually obtain popularization and application.Light according to coating
Degree, Acidic Sn electroplating can be divided into bright coating and half bright coating.The latter is also referred to as dark stannum, mist stannum and matte tin, compares the former, and half
Bright tin plating layer has excellent reliability, and it is suitable as the solderable coating of various electronic component, has more tin plating than entire bright
Preferably dispersibility, while taking into account assembly parts outward appearance needs, can reduce again the high light in installation to operator's eye
The stimulation in portion.
Conventional acidity half bright tin plating technique is divided into sulfuric acid type and sulfonic acid type two kinds.The latter's bath stability is good, electric current
Density is higher, is suitable for high speed electrodeposition and uses, but the cost of electroplate liquid is the highest.Comparatively speaking, although the former stability relatively
Low, but its low cost, and there is excellent covering power and dispersibility, the most leaded and other harmful substances in plating solution, at electricity
Sub-components and parts solderable coating and protectiveness coating are widely used.
Existing Technology Bright Acidic technology is highly developed, has a lot of pertinent literature to report both at home and abroad, and the document of half bright tin plating
Report the most less.Formula the most classical is that nineteen forty-one NACHTMAN discloses the continuous of a kind of strip steel at US2240265
Tin plating technique, its electroplate liquid consists of cresol sulfonic acid, betanaphthol and animal glue.The electroplate liquid of this patent is used till today always, is
The standard electric plating solution of currently used acquisition half light coating.Additionally, also minority half bright tin plating technique, be adapted to sulphuric acid-
Phenol sulfonic acid or pyrovinic acid system, the most rare about the half bright tin plating technique with sulphuric acid as disperse medium.Phenol sulfonic acid
There is the pollution problem of phenolic compound, therefore the plating solution as disperse medium is the most progressively eliminated.And metilsulfate body
It is that plating solution is relatively costly.Additionally, betanaphthol is still the main additive of existing half Bright Tin plating solution, but research shows, this material
Belong to the dangerous carcinogen of potentiality, thus preferably lack in electroplate liquid with or without.Accordingly, it would be desirable to exploitation does not use β-naphthalene
The half bright tin plating solution with sulphuric acid as disperse medium of phenol.
Summary of the invention
It is an object of the invention to provide a kind of acid half bright tin plating solution, the group of described acid half bright tin plating solution
Point and content be: stannous sulfate is 20-40g/L, and sulphuric acid is 80-110mL/L, benzylideneacetone be 0.1-0.5g/L, OP-10 be 2-
4mL/L, NP-10 are 1.5-3mL/L, and sodium benzoate is 0.9-1.5g/L, and nicotinic acid is 0.1-0.25g/L, and gelatin is 1-4g/L, sulfur
Acid ferrous iron is 2-3g/L, and ascorbic acid is 0.5-1g/L, and antimony potassium tartrate is 0.5-1g/L, and remaining is water.
Another object of the present invention is to provide the preparation method of described acid half bright tin plating solution, specifically include following
Step:
(1) being added to the water by sulphuric acid (98% concentrated sulphuric acid for commercially available), be cooled to room temperature, be subsequently adding stannous sulfate, stirring makes it
It is completely dissolved；
(2) nicotinic acid, gelatin and antimony potassium tartrate are added to the water so that it is be completely dissolved；
(3) sodium benzoate, ferrous sulfate and ascorbic acid are added to the water, and are sufficiently stirred for making it be completely dissolved；
(4) being joined by benzylideneacetone in the mixed solution of OP-10 and NP-10, stirring makes it be completely dissolved, and then add water stirring
Make it fully transparent, be cooled to room temperature afterwards；
(5) solution of step (2), (3), (4) gained is added in the solution of step (1) gained, be sufficiently stirred for making it mix all
Even, then adding water, it is volume required to be settled to, and i.e. obtains acid half bright tin plating solution.
Step (2) can heat water to 50 DEG C-60 DEG C to accelerate rate of dissolution.
With 50 DEG C of-60 DEG C of heating in water bath in course of dissolution in step (4).
Stannous sulfate of the present invention, sulphuric acid, benzylideneacetone, sodium benzoate, nicotinic acid, NP-10, OP-10, gelatin, sulphuric acid
Ferrous iron, ascorbic acid, antimony potassium tartrate are commercially available analytical pure chemical reagent.
Beneficial effects of the present invention: acid half bright tin plating solution solution dispersibility and covering power of the present invention
Good, operating temperature range and cathode-current density wide ranges, plating weldability is good, and adhesion is strong, and do not add carcinogen β-
Naphthols and poisonous aldehydes, to human body and environmentally friendly, and because institute's reagent adding is nontoxic, so raw material is easy to get and low price,
Reduce production cost to a certain extent.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described, but in the core without departing from the present invention
In the case of, any simple deformation, amendment or other those skilled in the art can not spend the equivalent of creative work to replace
Change and each fall within protection scope of the present invention.
Embodiment 1
Component and the content of the acid half bright tin plating solution of the present embodiment is: stannous sulfate 20g/L, sulphuric acid 80mL/L, benzal third
Ketone 0.1g/L, OP-10 2mL/L, NP-10 1.5mL/L, sodium benzoate 0.9g/L, nicotinic acid 0.1g/L, gelatin 1g/L, sulphuric acid is sub-
Ferrum 2g/L, ascorbic acid 0.5g/L, antimony potassium tartrate 0.5g/L, remaining is pure water.
In units of 1L, prepare acid half bright tin plating solution described in the present embodiment, specifically comprise the following steps that
(1) take a clean beaker, add 400mL pure water, take 80mL sulphuric acid and be slowly added in water, be cooled to room temperature.
(2) adding 20g stannous sulfate in step (1), stirring is to being completely dissolved.
(3) take a clean 10mL graduated cylinder, add NP-10 and the 0.1g benzylideneacetone of the OP-10,1.5mL of 2mL, 58
DEG C heating in water bath, adds after waiting benzylideneacetone to be completely dissolved in the beaker filling 100mL pure water, and 58 DEG C of heating in water bath are until it is complete
All-transparent, is cooled to room temperature afterwards.
(4) taking a clean beaker, add 20mL pure water, take 0.9g sodium benzoate and add in beaker, stirring is to the most molten
Solve.
(5) taking a clean beaker, add 30mL pure water, take 2g ferrous sulfate and add in beaker, stirring is to being completely dissolved.
(6) taking a clean beaker, add 50mL pure water, take 0.5g ascorbic acid and add in beaker, stirring is to the most molten
Solve.
(7) take a clean beaker, add 50mL pure water, take 0.1g nicotinic acid and add in beaker, 58 DEG C of heating in water bath, and stir
Mix and be completely dissolved to it, be cooled to room temperature afterwards.
(8) take a clean beaker, add 50mL pure water, take 1g gelatin and add in beaker, 58 DEG C of heating in water bath, and stir
It is completely dissolved to it, is cooled to room temperature afterwards.
(9) taking a clean beaker, add 50mL pure water, take 0.5g antimony potassium tartrate and add in beaker, 58 DEG C of water-baths add
Heat, and stir and be completely dissolved to it, it is cooled to room temperature afterwards.
(10) solution that step (3) (4) (5) (6) (7) (8) (9) obtains is joined in the solution that step (2) obtains, fill
Divide stirring to make its mix homogeneously, add water afterwards and be settled to 1L, i.e. obtain acid half bright tin plating solution.
This experiment is carried out in the Hull groove of 250mL, and the time is 5min, and anode is sheet tin, and negative electrode is copper sheet, electric current density
For 1A/dm2, temperature is room temperature.
Electrotinning technological process is:
Polishing → washing → pickling (30-50ml sulphuric acid/L, 10-15s) → wash → electroplate → wash → dry up.
Coating surface after the electroplate liquid plating prepared through the present embodiment is smooth, half light, without bubbling, pit and local nothing
The defects such as coating；Plating piece is impregnated in solder flux, then leaching 5s in the molten tin that temperature is 250 DEG C, surfacing after taking-up, 97%
Being stained with new tin layers (requiring >=95%), bubble-free and pin-hole phenomena, welding performance is good；Draw cutter with converted steel to draw on plating piece surface
Article two, at a distance of the parallel lines as deep as matrix for 2mm, the coating between two line does not come off, and adhesion is strong.
Embodiment 2
Component and the content of the acid half bright tin plating solution of the present embodiment is: stannous sulfate 40g/L, sulphuric acid 110mL/L, benzal third
Ketone 0.5g/L, OP-10 4mL/L, NP-10 3mL/L, sodium benzoate 1.5g/L, nicotinic acid 0.25g/L, gelatin 4g/L, ferrous sulfate
3g/L, ascorbic acid 1g/L, antimony potassium tartrate 1g/L, remaining is pure water.
In units of 1L, prepare acid half bright tin plating solution described in the present embodiment, specifically comprise the following steps that
(1) take a clean beaker, add 400mL pure water, take 110mL sulphuric acid and be slowly added in water, be cooled to room temperature.
(2) adding 20g stannous sulfate in step (1), stirring is to being completely dissolved.
(3) take a clean 10mL graduated cylinder, add OP-10 and the 0.5g benzylideneacetone of the NP-10,4mL of 3mL, 58 DEG C
Heating in water bath, adds after waiting benzylideneacetone to be completely dissolved in the beaker filling 100mL pure water, and 58 DEG C of heating in water bath are until it is complete
Transparent, it is cooled to room temperature afterwards.
(4) taking a clean beaker, add 20mL pure water, take 1.5g sodium benzoate and add in beaker, stirring is to the most molten
Solve.
(5) taking a clean beaker, add 30mL pure water, take 3g ferrous sulfate and add in beaker, stirring is to being completely dissolved.
(6) taking a clean beaker, add 50mL pure water, take 1g ascorbic acid and add in beaker, stirring is to being completely dissolved.
(7) take a clean beaker, add 50mL pure water, take 0.25g nicotinic acid and add in beaker, 58 DEG C of heating in water bath, and
Stirring is completely dissolved to it, is cooled to room temperature afterwards.
(8) take a clean beaker, add 50mL pure water, take 4g gelatin and add in beaker, 58 DEG C of heating in water bath, and stir
It is completely dissolved to it, is cooled to room temperature afterwards.
(9) take a clean beaker, add 50mL pure water, take 1g antimony potassium tartrate and add in beaker, 58 DEG C of heating in water bath,
And stir and be completely dissolved to it, it is cooled to room temperature afterwards.
(10) solution that step (3) (4) (5) (6) (7) (8) (9) obtains is joined in the solution that step (2) obtains, fill
Divide stirring to make its mix homogeneously, add water afterwards and be settled to 1L, i.e. obtain acid half bright tin plating solution.
This experiment is carried out in the Hull groove of 250mL, and the time is 5min, and anode is sheet tin, and negative electrode is copper sheet, electric current density
For 1A/dm2, temperature is room temperature.
Electrotinning technological process is:
Polishing → washing → pickling (30-50ml sulphuric acid/L, 10-15s) → wash → electroplate → wash → dry up.
Coating surface after the electroplate liquid plating prepared through the present embodiment is smooth, half light, without bubbling, pit and local nothing
The defects such as coating；Plating piece is impregnated in solder flux, then leaching 5s in the molten tin that temperature is 250 DEG C, surfacing after taking-up, 96%
Being stained with new tin layers (requiring >=95%), bubble-free and pin-hole phenomena, welding performance is good；Draw cutter with converted steel to draw on plating piece surface
Article two, at a distance of the parallel lines as deep as matrix for 2mm, the coating between two line does not come off, and adhesion is strong.
Embodiment 3
Component and the content of the acid half bright tin plating solution of the present embodiment is: stannous sulfate 30g/L, sulphuric acid 100mL/L, benzal third
Ketone 0.3g/L, OP-10 3mL/L, NP-10 2.5mL/L, sodium benzoate 1.2g/L, nicotinic acid 0.2g/L, gelatin 2g/L, sulphuric acid is sub-
Ferrum 2.5g/L, ascorbic acid 0.8g/L, antimony potassium tartrate 0.7g/L, remaining is pure water.
In units of 1L, prepare acid half bright tin plating solution described in the present embodiment, specifically comprise the following steps that
(1) take a clean beaker, add 400mL pure water, take 100mL sulphuric acid and be slowly added in water, be cooled to room temperature.
(2) adding 30g stannous sulfate in step (1), stirring is to being completely dissolved.
(3) take a clean 10mL graduated cylinder, add OP-10 and the 0.3g benzylideneacetone of the NP-10,3mL of 2.5mL, 58
DEG C heating in water bath, adds after waiting benzylideneacetone to be completely dissolved in the beaker filling 100mL pure water, and 58 DEG C of heating in water bath are until it is complete
All-transparent, is cooled to room temperature afterwards.
(4) taking a clean beaker, add 20mL pure water, take 1.2g sodium benzoate and add in beaker, stirring is to the most molten
Solve.
(5) taking a clean beaker, add 30mL pure water, take 2.5g ferrous sulfate and add in beaker, stirring is to the most molten
Solve.
(6) taking a clean beaker, add 50mL pure water, take 0.8g ascorbic acid and add in beaker, stirring is to the most molten
Solve.
(7) take a clean beaker, add 50mL pure water, take 0.2g nicotinic acid and add in beaker, 58 DEG C of heating in water bath, and stir
Mix and be completely dissolved to it, be cooled to room temperature afterwards.
(8) take a clean beaker, add 50mL pure water, take 2g gelatin and add in beaker, 58 DEG C of heating in water bath, and stir
It is completely dissolved to it, is cooled to room temperature afterwards.
(9) taking a clean beaker, add 50mL pure water, take 0.7g antimony potassium tartrate and add in beaker, 58 DEG C of water-baths add
Heat, and stir and be completely dissolved to it, it is cooled to room temperature afterwards.
(10) solution that step (3) (4) (5) (6) (7) (8) (9) obtains is joined in the solution that step (2) obtains, fill
Divide stirring to make its mix homogeneously, add water afterwards and be settled to 1L, i.e. obtain acid half bright tin plating solution.
This experiment is carried out in the Hull groove of 250mL, and the time is 5min, and anode is sheet tin, and negative electrode is copper sheet, electric current density
For 1A/dm2, temperature is room temperature.
Electrotinning technological process is:
Polishing → washing → pickling (30-50ml sulphuric acid/L, 10-15s) → wash → electroplate → wash → dry up.
Coating surface after the electroplate liquid plating prepared through the present embodiment is smooth, half light, without bubbling, pit and local nothing
The defects such as coating；Plating piece is impregnated in solder flux, then leaching 5s in the molten tin that temperature is 250 DEG C, surfacing after taking-up, 99%
Being stained with new tin layers (requiring >=95%), bubble-free and pin-hole phenomena, welding performance is good；Draw cutter with converted steel to draw on plating piece surface
Article two, at a distance of the parallel lines as deep as matrix for 2mm, the coating between two line does not come off, and adhesion is strong.
Claims (2)
1. an acidity half bright tin plating solution, it is characterised in that: component and the content of described acid half bright tin plating solution is:
Stannous sulfate is 20-40g/L, and sulphuric acid is 80-110mL/L, benzylideneacetone be 0.1-0.5g/L, OP-10 be 2-4mL/L, NP-10
For 1.5-3mL/L, sodium benzoate is 0.9-1.5g/L, and nicotinic acid is 0.1-0.25g/L, and gelatin is 1-4g/L, and ferrous sulfate is 2-
3g/L, ascorbic acid is 0.5-1g/L, and antimony potassium tartrate is 0.5-1g/L, and remaining is water.
2. the preparation method of an acid half bright tin plating solution as claimed in claim 1, it is characterised in that specifically include following
Step:
(1) being added to the water by sulphuric acid, be cooled to room temperature, be subsequently adding stannous sulfate, stirring makes it be completely dissolved；
(2) nicotinic acid, gelatin and antimony potassium tartrate are added to the water so that it is be completely dissolved；
(3) sodium benzoate, ferrous sulfate and ascorbic acid are added to the water, and are sufficiently stirred for making it be completely dissolved；
(4) being joined by benzylideneacetone in the mixed solution of OP-10 and NP-10, stirring makes it be completely dissolved, and then add water stirring
Make it fully transparent, be cooled to room temperature afterwards；
(5) solution of step (2), (3), (4) gained is added in the solution of step (1) gained, be sufficiently stirred for making it mix all
Even, then adding water, it is volume required to be settled to, and i.e. obtains acid half bright tin plating solution.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835210A (en) * | 2017-03-09 | 2017-06-13 | 昆明理工大学 | A kind of sulfate bright tin plating solution and preparation method thereof |
| CN108396343A (en) * | 2018-05-05 | 2018-08-14 | 深圳市竑鎏电子表面处理科技有限公司 | A kind of mist tin additive and the electroplate liquid using the mist tin additive |
| TWI703239B (en) * | 2018-03-20 | 2020-09-01 | 日商三菱綜合材料股份有限公司 | Plating solution of tin or tin alloy and method for forming bumps |
| CN113430593A (en) * | 2021-05-10 | 2021-09-24 | 江苏灏润新材料科技有限公司 | Novel additive suitable for high-speed copper-tin composite production |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3483100A (en) * | 1966-09-14 | 1969-12-09 | Philips Corp | Tin plating baths |
| JPS58151487A (en) * | 1982-03-01 | 1983-09-08 | Shinko Electric Ind Co Ltd | Tin electroplating bath made acidic with hydrochloric aicd |
| US4439286A (en) * | 1981-07-14 | 1984-03-27 | Edinen Centar Po Chimia | Electrolyte for the deposition of bright tin coatings |
| JPH0754184A (en) * | 1993-08-17 | 1995-02-28 | Kobe Steel Ltd | Sulfuric acid tin plating bath for reflow plating capable of embodying fast continuous plating |
| CN101922026A (en) * | 2010-08-18 | 2010-12-22 | 济南德锡科技有限公司 | Methanesulfonic acid-based matte pure tin electroplating solution and additive thereof |
| CN101962790A (en) * | 2010-08-20 | 2011-02-02 | 河南科技大学 | Electrolyte composition for half bright acid tinning |
| CN103882485A (en) * | 2014-04-04 | 2014-06-25 | 哈尔滨工业大学 | All-sulfate tin electroplating additive and plating solution thereof |
| CN105063680A (en) * | 2015-08-21 | 2015-11-18 | 无锡桥阳机械制造有限公司 | Sulfonic acid type semi-bright pure-tin electroplating liquid |
| CN105648483A (en) * | 2016-04-11 | 2016-06-08 | 济南德锡科技有限公司 | High-speed tinning solution and preparation method thereof |
-
2016
- 2016-08-29 CN CN201610742278.5A patent/CN106222710A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3483100A (en) * | 1966-09-14 | 1969-12-09 | Philips Corp | Tin plating baths |
| US4439286A (en) * | 1981-07-14 | 1984-03-27 | Edinen Centar Po Chimia | Electrolyte for the deposition of bright tin coatings |
| JPS58151487A (en) * | 1982-03-01 | 1983-09-08 | Shinko Electric Ind Co Ltd | Tin electroplating bath made acidic with hydrochloric aicd |
| JPH0754184A (en) * | 1993-08-17 | 1995-02-28 | Kobe Steel Ltd | Sulfuric acid tin plating bath for reflow plating capable of embodying fast continuous plating |
| CN101922026A (en) * | 2010-08-18 | 2010-12-22 | 济南德锡科技有限公司 | Methanesulfonic acid-based matte pure tin electroplating solution and additive thereof |
| CN101962790A (en) * | 2010-08-20 | 2011-02-02 | 河南科技大学 | Electrolyte composition for half bright acid tinning |
| CN103882485A (en) * | 2014-04-04 | 2014-06-25 | 哈尔滨工业大学 | All-sulfate tin electroplating additive and plating solution thereof |
| CN105063680A (en) * | 2015-08-21 | 2015-11-18 | 无锡桥阳机械制造有限公司 | Sulfonic acid type semi-bright pure-tin electroplating liquid |
| CN105648483A (en) * | 2016-04-11 | 2016-06-08 | 济南德锡科技有限公司 | High-speed tinning solution and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张立茗等: "《实用电镀添加剂》", 31 January 2007, 化学工业出版社 * |
| 曾华樑等: "《电镀技术问题对策》", 31 October 2006, 机械工业出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835210A (en) * | 2017-03-09 | 2017-06-13 | 昆明理工大学 | A kind of sulfate bright tin plating solution and preparation method thereof |
| TWI703239B (en) * | 2018-03-20 | 2020-09-01 | 日商三菱綜合材料股份有限公司 | Plating solution of tin or tin alloy and method for forming bumps |
| US11053600B2 (en) | 2018-03-20 | 2021-07-06 | Mitsubishi Materials Corporation | Tin or tin alloy plating solution and bump forming method |
| CN108396343A (en) * | 2018-05-05 | 2018-08-14 | 深圳市竑鎏电子表面处理科技有限公司 | A kind of mist tin additive and the electroplate liquid using the mist tin additive |
| CN113430593A (en) * | 2021-05-10 | 2021-09-24 | 江苏灏润新材料科技有限公司 | Novel additive suitable for high-speed copper-tin composite production |
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