CN113684508A - Compacting agent for neutral electrotinning, electroplating solution containing compacting agent, preparation method and application thereof - Google Patents
Compacting agent for neutral electrotinning, electroplating solution containing compacting agent, preparation method and application thereof Download PDFInfo
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- CN113684508A CN113684508A CN202111028207.6A CN202111028207A CN113684508A CN 113684508 A CN113684508 A CN 113684508A CN 202111028207 A CN202111028207 A CN 202111028207A CN 113684508 A CN113684508 A CN 113684508A
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- polyethylene glycol
- agent
- neutral
- sulfonic acid
- water
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- 230000007935 neutral effect Effects 0.000 title claims abstract description 31
- 238000009713 electroplating Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 26
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 26
- 150000004782 1-naphthols Chemical class 0.000 claims abstract description 22
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 33
- 238000000280 densification Methods 0.000 claims description 29
- 229940113116 polyethylene glycol 1000 Drugs 0.000 claims description 20
- 238000007747 plating Methods 0.000 claims description 16
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- AICMYQIGFPHNCY-UHFFFAOYSA-J methanesulfonate;tin(4+) Chemical compound [Sn+4].CS([O-])(=O)=O.CS([O-])(=O)=O.CS([O-])(=O)=O.CS([O-])(=O)=O AICMYQIGFPHNCY-UHFFFAOYSA-J 0.000 claims description 6
- 239000013078 crystal Substances 0.000 abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052759 nickel Inorganic materials 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 239000006258 conductive agent Substances 0.000 description 5
- 238000012876 topography Methods 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 1
- 238000011990 functional testing Methods 0.000 description 1
- -1 hydroxy acid salt Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses a compacting agent for neutral electrotinning, an electroplating solution containing the compacting agent, a preparation method and an application thereof, wherein the compacting agent comprises the following components in percentage by mass: 20-30% of ethoxylated alpha-naphthol sulfonic acid, 100010-20% of polyethylene glycol, 60005-15% of polyethylene glycol and the balance of water. The invention provides a compacting agent for neutral electrolytic tinning, which can effectively prevent a nickel layer from being oxidized, and has compact crystals and excellent effect.
Description
Technical Field
The invention relates to the technical field of electroplating, in particular to a compacting agent for neutral electrotinning, an electroplating solution containing the compacting agent, and a preparation method and application of the electroplating solution.
Background
At present, under the miniaturization trend and on the premise of keeping reliable functionality of electronic products, a metallic tin layer is still needed to be plated on the products in an electrochemical mode to keep weldability, so that the miniature products such as chip resistors (chip-resistors), multi-layer capacitor (multi-layer capacitor) and chip inductors (chip-inductors) and the like must use a neutral tin plating system, the electroplating chemicals can avoid the products from being stuck together during electroplating, and the electroplated tin crystal densification agent plays a key role in functional test, because the nickel layer can be prevented from being oxidized only when the crystals are densified, and the electronic products cannot perform the welding function and can only be scrapped if the nickel layer is oxidized.
In conclusion, in electronic products, a problem that how to provide a novel neutral electroplated tin crystal densification agent is a problem that needs to be solved is to be solved because an effective densification agent for preventing nickel layer from being oxidized is lacked.
Disclosure of Invention
Therefore, the invention provides a compacting agent for neutral electroplating tin, an electroplating solution containing the compacting agent, and a preparation method and application thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a compacting agent for neutral electrolytic tinning, which comprises the following components in percentage by mass: 20-30% of ethoxylated alpha-naphthol sulfonic acid, 100010-20% of polyethylene glycol, 60005-15% of polyethylene glycol and the balance of water.
In one embodiment of the invention, the densification agent comprises the following components in percentage by mass: 21-29% of ethoxylated alpha-naphthol sulfonic acid, 100011-19% of polyethylene glycol, 60006-14% of polyethylene glycol and the balance of water.
In one embodiment of the invention, the densification agent comprises the following components in percentage by mass: 25% of ethoxylated alpha-naphthol sulfonic acid, 100015% of polyethylene glycol, 600010% of polyethylene glycol and the balance of water.
The invention also comprises a method for preparing the compacting agent for neutral electrolytic tinning, which comprises the following components in proportion: water, ethoxylated alpha-naphthol sulfonic acid, polyethylene glycol 1000, polyethylene glycol 6000;
adding 50% by mass of water into a container and stirring;
adding said polyethylene glycol 1000 to said stirred water to form a polyethylene glycol 1000 solution;
adding polyethylene glycol 6000 into the polyethylene glycol 1000 solution, and stirring for 0.5-1.5h to obtain a mixed solution;
and adding the rest water and the ethoxylated alpha-naphthol sulfonic acid into the mixed solution, and stirring for 3.5-4.5h to obtain the compacting agent for neutral electrolytic tinning.
In one embodiment of the invention, the stirring speed is 10-20 r/min.
In one embodiment of the invention, the components are calculated by mass percent: 20-30% of ethoxylated alpha-naphthol sulfonic acid, 100010-20% of polyethylene glycol, 60005-15% of polyethylene glycol and the balance of water.
The embodiment of the invention provides an electroplating solution and a densification agent prepared by the method.
In one embodiment of the present invention, the plating solution further comprises tin methane sulfonate.
The invention has the following advantages:
the invention provides a compacting agent for neutral electrolytic tinning, which can effectively prevent a nickel layer from being oxidized, and has compact crystals and excellent effect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
FIG. 1 is a photograph of a scanning electron microscope examination of the surface topography of a barrel-plated product of an electroplating solution containing a densification agent of example 1 after steam aging in accordance with an embodiment of the present invention;
FIG. 2 is a photograph of a scanning electron microscope examination of the surface topography of a barrel-plated product of an electroplating solution containing a densification agent of example 2 after steam aging in accordance with an embodiment of the present invention;
FIG. 3 is a photograph of a scanning electron microscope examination of the surface topography of a vapor aged barrel-plated product of an electroplating solution containing a densification agent of example 3 provided in accordance with an embodiment of the present invention;
FIG. 4 is a photograph of a scanning electron microscope examination of the surface topography of a vapor aged barrel-plated product of an electroplating solution containing a densification agent of example 4 in accordance with an embodiment of the present invention;
FIG. 5 is a photograph of a scanning electron microscope examination of the surface topography of a barrel-plated product of an electroplating solution containing a prior densification agent after steam aging, according to an embodiment of the present invention.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present invention, the molecular formula of the ethoxylated alpha-naphthol sulfonic acid is as shown in formula (I)
Example 1
The preparation method of the densification agent for neutral electrolytic tinning provided by the embodiment comprises the following steps of:
step one, weighing 100010% of polyethylene glycol, 60005% of polyethylene glycol, 20% of ethoxylated alpha-naphthol sulfonic acid and 65% of pure water according to mass fraction;
step two, adding pure water into the stirring tank and starting stirring, wherein the stirring speed is 10-20 r/min;
step three, slowly adding polyethylene glycol 1000 into pure water, and uniformly stirring to obtain a polyethylene glycol 1000 solution;
step four, slowly adding polyethylene glycol 6000 into the polyethylene glycol 1000 solution, and slowly stirring for 1h at the stirring speed of 10-20r/min to obtain a mixed solution;
step five, adding ethoxylated alpha-naphthol sulfonic acid into the mixed solution, and continuously stirring for 4 hours at the stirring speed of 10-20r/min to obtain the compacting agent for neutral electrolytic tinning
Example 2
The preparation method of the densification agent for neutral electrolytic tinning provided by the embodiment comprises the following steps of:
step one, weighing 100020% of polyethylene glycol, 600015% of polyethylene glycol, 30% of ethoxylated alpha-naphthol sulfonic acid and 35% of pure water according to mass fraction;
step two, adding pure water into the stirring tank and starting stirring, wherein the stirring speed is 10-20 r/min;
step three, slowly adding polyethylene glycol 1000 into pure water, and uniformly stirring to obtain a polyethylene glycol 1000 solution;
step four, slowly adding polyethylene glycol 6000 into the polyethylene glycol 1000 solution, and slowly stirring for 1h at the stirring speed of 10-20r/min to obtain a mixed solution;
and step five, adding the ethoxylated alpha-naphthol sulfonic acid into the mixed solution, and continuously stirring for 4 hours at the stirring speed of 10-20r/min to obtain the compacting agent for neutral electrolytic tinning.
Example 3
The preparation method of the densification agent for neutral electrolytic tinning provided by the embodiment comprises the following steps of:
step one, weighing 100015% of polyethylene glycol, 600010% of polyethylene glycol, 25% of ethoxylated alpha-naphthol sulfonic acid and 50% of pure water according to mass fraction;
step two, adding pure water into the stirring tank and starting stirring, wherein the stirring speed is 10-20 r/min;
step three, slowly adding polyethylene glycol 1000 into pure water, and uniformly stirring to obtain a polyethylene glycol 1000 solution;
step four, slowly adding polyethylene glycol 6000 into the polyethylene glycol 1000 solution, and slowly stirring for 1h at the stirring speed of 10-20r/min to obtain a mixed solution;
and step five, adding the ethoxylated alpha-naphthol sulfonic acid into the mixed solution, and continuously stirring for 4 hours at the stirring speed of 10-20r/min to obtain the compacting agent for neutral electrolytic tinning.
Example 4
The preparation method of the densification agent for neutral electrolytic tinning provided by the embodiment comprises the following steps of:
step one, weighing 100015% of polyethylene glycol, 600010% of polyethylene glycol, 30% of ethoxylated alpha-naphthol sulfonic acid and 45% of pure water according to mass fraction;
step two, adding pure water into the stirring tank and starting stirring, wherein the stirring speed is 10-20 r/min;
step three, slowly adding polyethylene glycol 1000 into pure water, and uniformly stirring to obtain a polyethylene glycol 1000 solution;
step four, slowly adding polyethylene glycol 6000 into the polyethylene glycol 1000 solution, and slowly stirring for 1h at the stirring speed of 10-20r/min to obtain a mixed solution;
and step five, adding the ethoxylated alpha-naphthol sulfonic acid into the mixed solution, and continuously stirring for 4 hours at the stirring speed of 10-20r/min to obtain the compacting agent for neutral electrolytic tinning.
Test examples
The test method of the test embodiment of the invention is as follows:
preparing tin methane sulfonate (Sn) with the same concentration2+12g/L), 250ml/L of tin plating conductive agent and 50ml/L of neutral electroplating tin densification agent. The tin plating conductive agent is prepared from the following components in percentage by mass: 20% of hydroxy acid salt, 15% of sodium hydroxide and 65% of pure water.
A plating solution was prepared by mixing 40ml/L (4%) by volume of tin methanesulfonate, 250ml/L (25%) by volume of a tin plating conductive agent and 50ml/L (5%) by volume of the neutral tin plating crystal densification agent obtained in examples 1 to 4 of the present invention.
In the above preparation, 40ml/L (4%) of tin methanesulfonate means that 40ml of tin methanesulfonate solution was contained in 1L of the mixed solution;
250ml/L (25%) of tin plating conductive agent refers to that 250ml of tin plating conductive agent solution is contained in 1L of mixed solution;
50ml/L (5%) of the neutral tin-plated crystal densification agent means that 50ml of the neutral densification agent of example 1 or example 2 or example 3 or example 4 is contained in 1L of the mixed solution.
And using a plating solution prepared by a same method with a commercially available common crystal densification agent as a comparative example, adjusting the pH value to 3.5(pH 3.5) with 5% of the commercially available common crystal densification agent, and miniaturizing three main flow passive components in a certain amount: the 0402 chip resistor is barrel-plated in the prepared electroplating solution for 90 minutes at 0.5ASD (ampere/square decimeter), and each batch is subjected to 1000 grains for 4 hours, 1000 grains for 8 hours and 1000 grains for 16 hours for direct SMT (surface mount technology) and the surface morphology is detected by 3000 times of a Scanning Electron Microscope (SEM). The results are shown in Table 1.
TABLE 1
As shown in fig. 1 to 4, photographs of the surface morphology of the barrel-plated product of the electroplating solution containing the densification agent of the present invention after steam aging by a Scanning Electron Microscope (SEM) show crystal densification; fig. 5 is a photograph showing the surface morphology of the comparative example measured by a Scanning Electron Microscope (SEM), showing that the crystals are loose. Experiments prove that the neutral tin-plating novel crystal compacting agent can prevent a nickel layer from being oxidized, and has compact crystals and very good effect.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. A densification agent for neutral electrolytic tinning is characterized in that,
the densification agent comprises the following components in percentage by mass: 20-30% of ethoxylated alpha-naphthol sulfonic acid, 100010-20% of polyethylene glycol, 60005-15% of polyethylene glycol and the balance of water.
2. The densification agent for neutral electrolytic tin plating according to claim 1, wherein,
the densification agent comprises the following components in percentage by mass: 21-29% of ethoxylated alpha-naphthol sulfonic acid, 100011-19% of polyethylene glycol, 60006-14% of polyethylene glycol and the balance of water.
3. The densification agent for neutral electrolytic tin plating according to claim 1, wherein,
the densification agent comprises the following components in percentage by mass: 25% of ethoxylated alpha-naphthol sulfonic acid, 100015% of polyethylene glycol, 600010% of polyethylene glycol and the balance of water.
4. A method for preparing the compacting agent for neutral electrolytic tinning according to any of claims 1 to 3,
taking the following components in proportion: water, ethoxylated alpha-naphthol sulfonic acid, polyethylene glycol 1000, polyethylene glycol 6000;
adding 50% by mass of water into a container and stirring;
adding said polyethylene glycol 1000 to said stirred water to form a polyethylene glycol 1000 solution;
adding polyethylene glycol 6000 into the polyethylene glycol 1000 solution, and stirring for 0.5-1.5h to obtain a mixed solution;
and adding the rest water and the ethoxylated alpha-naphthol sulfonic acid into the mixed solution, and stirring for 3.5-4.5h to obtain the compacting agent for neutral electrolytic tinning.
5. The method of claim 4,
the stirring speed is 10-20 r/min.
6. The method of claim 4,
the components are calculated by mass percent: 20-30% of ethoxylated alpha-naphthol sulfonic acid, 100010-20% of polyethylene glycol, 60005-15% of polyethylene glycol and the balance of water.
7. An electroplating solution comprising the neutral electrolytic tin plating densifying agent prepared by the method of any one of claims 4 to 6.
8. The plating solution according to claim 7,
the plating solution also includes tin methane sulfonate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111028207.6A CN113684508A (en) | 2021-09-02 | 2021-09-02 | Compacting agent for neutral electrotinning, electroplating solution containing compacting agent, preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111028207.6A CN113684508A (en) | 2021-09-02 | 2021-09-02 | Compacting agent for neutral electrotinning, electroplating solution containing compacting agent, preparation method and application thereof |
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| CN113684508A true CN113684508A (en) | 2021-11-23 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05156488A (en) * | 1991-12-05 | 1993-06-22 | Nippon Steel Corp | Acidic sn plating bath reduced in deposition of sn sludge |
| WO1997023664A1 (en) * | 1995-12-22 | 1997-07-03 | Toyo Kohan Co., Ltd. | Tinning bath and tinning method |
| CN109594107A (en) * | 2018-11-13 | 2019-04-09 | 南通赛可特电子有限公司 | A kind of electrotinning additive and preparation method thereof |
| CN110106535A (en) * | 2019-06-10 | 2019-08-09 | 广东比格莱科技有限公司 | A kind of tin plating additive of neutrality |
| CN110205659A (en) * | 2019-07-17 | 2019-09-06 | 广州三孚新材料科技股份有限公司 | Electrotinning additive and preparation method thereof |
-
2021
- 2021-09-02 CN CN202111028207.6A patent/CN113684508A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05156488A (en) * | 1991-12-05 | 1993-06-22 | Nippon Steel Corp | Acidic sn plating bath reduced in deposition of sn sludge |
| WO1997023664A1 (en) * | 1995-12-22 | 1997-07-03 | Toyo Kohan Co., Ltd. | Tinning bath and tinning method |
| CN109594107A (en) * | 2018-11-13 | 2019-04-09 | 南通赛可特电子有限公司 | A kind of electrotinning additive and preparation method thereof |
| CN110106535A (en) * | 2019-06-10 | 2019-08-09 | 广东比格莱科技有限公司 | A kind of tin plating additive of neutrality |
| CN110205659A (en) * | 2019-07-17 | 2019-09-06 | 广州三孚新材料科技股份有限公司 | Electrotinning additive and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 方景礼: "《电镀添加剂理论与应用》", 30 April 2006, 国防工业出版社 * |
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