CN114808051A - Tin plating solution for magnetic core inductance electroplating and preparation method thereof - Google Patents
Tin plating solution for magnetic core inductance electroplating and preparation method thereof Download PDFInfo
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- CN114808051A CN114808051A CN202111219185.1A CN202111219185A CN114808051A CN 114808051 A CN114808051 A CN 114808051A CN 202111219185 A CN202111219185 A CN 202111219185A CN 114808051 A CN114808051 A CN 114808051A
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- 238000007747 plating Methods 0.000 title claims abstract description 97
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000009713 electroplating Methods 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 48
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims abstract description 38
- -1 alkyl compound Chemical class 0.000 claims abstract description 37
- 150000003839 salts Chemical class 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 22
- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical compound [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000007513 acids Chemical class 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 15
- 235000015165 citric acid Nutrition 0.000 claims description 13
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 12
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 12
- 239000000176 sodium gluconate Substances 0.000 claims description 12
- 229940005574 sodium gluconate Drugs 0.000 claims description 12
- 235000012207 sodium gluconate Nutrition 0.000 claims description 12
- 239000011975 tartaric acid Substances 0.000 claims description 12
- 235000002906 tartaric acid Nutrition 0.000 claims description 12
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 10
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000174 gluconic acid Substances 0.000 claims description 8
- 235000012208 gluconic acid Nutrition 0.000 claims description 8
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 150000001450 anions Chemical class 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 239000001433 sodium tartrate Substances 0.000 claims description 3
- 229960002167 sodium tartrate Drugs 0.000 claims description 3
- 235000011004 sodium tartrates Nutrition 0.000 claims description 3
- WPUMTJGUQUYPIV-JIZZDEOASA-L disodium (S)-malate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](O)CC([O-])=O WPUMTJGUQUYPIV-JIZZDEOASA-L 0.000 claims description 2
- 235000019265 sodium DL-malate Nutrition 0.000 claims description 2
- 229960001790 sodium citrate Drugs 0.000 claims description 2
- 235000011083 sodium citrates Nutrition 0.000 claims description 2
- 239000001394 sodium malate Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 239000012535 impurity Substances 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- 239000006260 foam Substances 0.000 abstract description 3
- 238000005476 soldering Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 239000011248 coating agent Substances 0.000 description 11
- 238000000576 coating method Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 7
- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 description 6
- JALQQBGHJJURDQ-UHFFFAOYSA-L bis(methylsulfonyloxy)tin Chemical compound [Sn+2].CS([O-])(=O)=O.CS([O-])(=O)=O JALQQBGHJJURDQ-UHFFFAOYSA-L 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 4
- KKVTYAVXTDIPAP-UHFFFAOYSA-M sodium;methanesulfonate Chemical group [Na+].CS([O-])(=O)=O KKVTYAVXTDIPAP-UHFFFAOYSA-M 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005338 heat storage Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 1
- 229910020938 Sn-Ni Inorganic materials 0.000 description 1
- 229910008937 Sn—Ni Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000006177 alkyl benzyl group Chemical group 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- VICYBMUVWHJEFT-UHFFFAOYSA-N dodecyltrimethylammonium ion Chemical compound CCCCCCCCCCCC[N+](C)(C)C VICYBMUVWHJEFT-UHFFFAOYSA-N 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- KKWUACQXLWHLCX-UHFFFAOYSA-N hydron;tetradecan-1-amine;chloride Chemical compound Cl.CCCCCCCCCCCCCCN KKWUACQXLWHLCX-UHFFFAOYSA-N 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- XWIJIXWOZCRYEL-UHFFFAOYSA-M potassium;methanesulfonate Chemical compound [K+].CS([O-])(=O)=O XWIJIXWOZCRYEL-UHFFFAOYSA-M 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/001—Magnets
Landscapes
- 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 tin plating solution for magnetic core inductance electroplating and a preparation method thereof, wherein the tin plating solution comprises the following components: (1) at least one salt of a hydroxycarboxylic acid; (2) at least two polycarboxylic acids; (3) at least one stannous ion source; (4) at least one salt substance; (5) at least one C10-C14 alkyl compound. The preparation method comprises the steps of adding the hydroxyl carboxylate, the salt substance and the polycarboxylic acid into deionized water, stirring and dissolving, adding the stannous ion source, and continuously stirring uniformly; and finally adding a C10-C14 alkyl compound to obtain the product. The plating solution of the system has good stability, white and bright appearance of the plating layer, compact and uniform appearance, steam corrosion resistance, less impurities and excellent soldering tin performance, and the low-foam environment-friendly tin plating solution is convenient for cleaning the plated product and has longer quality guarantee period. In addition, most of the materials used by the tin plating solution are food-grade materials or environment-friendly materials, so that the tin plating solution has low harm to human bodies and little pollution to the environment, and the operation of workers does not need strict protection.
Description
Technical Field
The invention relates to the field of preparation of tin plating solution, C25D3/32, in particular to tin plating solution for magnetic core inductance electroplating and a preparation method thereof.
Background
The inductor is an important electronic component, has wide application in various electronic circuits, and brings convenience for realizing various electronic functions. The magnetic core is made of materials with higher magnetic permeability than air, and can restrain a magnetic field around the inductance device more tightly to increase inductance. The magnetic core inductor has important energy storage, filtering and oscillation functions, and the inductor assembly is required to be welded with a circuit through wave soldering to be integrated after being mounted on an inductor assembly patch. In order to improve the solderability of the inductor assembly, it is often necessary to subject the inductor assembly to an electroplating process. The tin coating is as outmost cladding material, plays the effect of protection inlayer cladding material not oxidized, replaces the good welding performance of subassembly simultaneously.
Patent CN105648483 discloses a high-speed tin plating solution and a preparation method thereof, wherein the growth of tin whiskers is strictly limited by the combination of three grain refiners, uniform plating layers can be generated in different current densities, and meanwhile, the use of a low-foaming surfactant is used to reduce plating layer impurities and avoid the use of a defoaming agent, so that the discoloration resistance of the plating layer is ensured. Patent CN110306213 proposes a tin plating solution for solar cells and a preparation method thereof, the tin plating solution includes: the composite coating is characterized in that the composite coating is prepared by combining methyl sulfonic acid, stannous methanesulfonate, an accelerant, a stabilizer, water, an accelerant composed of palmitoyl methionine and acetylene compounds and a stabilizer composed of reducing saccharide compounds and sodium citrate, so that the bonding force between a stable coating of the tin plating solution and a matrix is improved, and the final coating is flat, uniform and compact and meets the requirements of a solar photovoltaic module. However, the preparation process of the tin plating solution is complex, low-current electrolytic treatment needs to be carried out for 2 to 4 hours after the tin plating solution is uniformly stirred and is circularly filtered for 2 to 5 times, and the required time is long. Therefore, the research on the tin plating solution for the magnetic core inductance electroplating, which has the advantages of good stability and simple preparation process, is of great significance, and the tin plating solution also has the characteristics of uniform and compact appearance of a plating layer, steam corrosion resistance, less impurities and excellent weldability.
Disclosure of Invention
In order to solve the above problems, the first aspect of the present invention provides a tin plating solution for magnetic core inductance electroplating: the method comprises the following steps:
(1) at least one salt of a hydroxycarboxylic acid;
(2) at least two polycarboxylic acids;
(3) at least one stannous ion source;
(4) at least one salt-like substance, wherein the anion of the salt-like substance is the same as the anion of the stannous ion source;
(5) at least one C10-C14 alkyl compound;
wherein: the hydroxycarboxylic acid salt is different from the polycarboxylic acid in the carboxylate ion, and the number of hydroxyl groups of the hydroxycarboxylic acid salt is not less than the number of hydroxyl groups of the polycarboxylic acid.
By adding hydroxyl carboxylate and polycarboxylic acid into the stannous methanesulfonate plating solution, the content of stannous ions in the plating solution can reach 5-15g/L, thereby realizing high-speed plating; however, in the development process, developers find that if the hydroxyl carboxylate and the polycarboxylic acid are not selected properly, the carboxylate is combined with hydrogen in the plating solution in a large amount to reduce the plating efficiency, so that the developers tend to replace the hydroxyl carboxylate or the polycarboxylic acid with other substances. But the method can bring the problem of poor stability of the plating solution, for example, turbidity appears when the plating is continuously carried out for no more than 40 days in the electroplating process, and the service life of the plating solution is seriously influenced.
Due to the development trend of environmental protection, research personnel strive to realize excellent tin plating by using food-grade materials or environment-friendly materials, reduce harm to human bodies, have little pollution to the environment and do not need strict protection for staff operation; the present inventors have found that when the carboxylate salt is different from the carboxylate ion of the polycarboxylic acid; when the number of the hydroxyl groups of the hydroxycarboxylic acid salt is more than or equal to that of the polycarboxylic acid, the salt substances are combined, and the C10-C14 alkyl compounds are cooperated with each other, so that the pH value of the plating solution is stabilized at 3-5; the stability of current in the electroplating process is ensured, and the magnetic core inductance in the electroplating process can not be burnt; and the hydroxyl carboxylate is sodium gluconate, so that when the polycarboxylic acid is citric acid or tartaric acid, an antioxidant is not required to be added, and the tin plating solution is continuously plated for more than 65 days in the electroplating process without turbidity.
The hydroxyl carboxylate is selected from at least one of sodium gluconate, sodium citrate, sodium tartrate and sodium malate;
the polycarboxylic acid is selected from at least two of gluconic acid, citric acid, tartaric acid and malic acid;
in a preferred embodiment, the salt of a hydroxycarboxylic acid is sodium gluconate, the first polycarboxylic acid is gluconic acid, and the second polycarboxylic acid is citric acid; or the hydroxyl carboxylate is sodium gluconate, the first polycarboxylic acid is tartaric acid, and the second polycarboxylic acid is gluconic acid; or the hydroxyl carboxylate is sodium gluconate, the first polycarboxylic acid is tartaric acid, and the second polycarboxylic acid is citric acid;
in a preferred embodiment, the salt of hydroxycarboxylic acid is sodium tartrate, then the polycarboxylic acid is citric acid, malic acid;
the stannous ion source is stannous methanesulfonate;
the salt substance is sodium methanesulfonate and/or potassium methanesulfonate;
the C10-C14 alkyl compound is selected from at least one of dodecyl trimethyl ammonium, dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride, sodium dodecyl benzene sulfonate, dodecyl trimethyl ammonium chloride, trimethyl tetradecyl ammonium chloride and tetradecyl ammonium chloride; preferably, the C10-C14 alkyl compound is a C10-C14 alkyl benzyl compound; more preferably, the C10-C14 alkyl benzyl compound is dodecyl dimethyl benzyl ammonium chloride;
by adding a C10-C14 alkyl compound to the plating solution, the C10-C14 alkyl compound selectively adsorbs on the unevenness of the electrode surface, thereby promoting uniform deposition of tin; however, if the hydroxyl carboxylate and the polycarboxylic acid are not selected reasonably, the oxidation resistance and the steam resistance of the coating are poor; the reason is that the hydroxycarboxylic acid and the polycarboxylic acid influence the selective adsorption of the C10-C14 alkyl compound; research of research personnel discovers that when the polycarboxylic acid is citric acid or tartaric acid, the steam resistance of the coating is improved; particularly, the C10-C14 alkyl compound is a C10-C14 alkyl benzyl compound, the plating layer does not change color after resisting water vapor for 16 hours at the electroplating temperature of 22-30 ℃, the oxidation resistance is strong, and the appearance of the tin plating layer is white and bright; supposing that the chain head of the C10-C14 alkyl benzyl compound is adsorbed on the surface of the electrode, the chain tail is dissociated on the surface of the electrode, and the proper electroplating temperature increases the proportion of the chain head functional group in the adsorption, so that the selection effect is more obvious, and the crystal grains are finer; after the temperature is increased, the thermal movement increases the influence of the selective adsorption of the hydroxycarboxylic acid salts, polycarboxylic acids on the C10-C14 alkyl compounds, while the selectivity of the C10-C14 alkylbenzyl compounds themselves decreases.
Preferably, the mass concentration of the hydroxycarboxylic acid salt is 50-100 g/L;
preferably, the mass concentration of the polycarboxylic acid is 9-18 g/L;
preferably, the mass concentration ratio of the first polycarboxylic acid to the second polycarboxylic acid is 0.6-1.3: 1;
preferably, the mass concentration of the stannous ion source is 5-15 g/L;
preferably, the mass concentration of the salt substance is 30-100 g/L; more preferably 30 to 50 g/L;
preferably, the mass concentration of the C10-C14 alkyl compound is 1-5 g/L.
The pH value of the tin plating solution is 3-5.
The electroplating conditions of the tin plating solution are as follows: the temperature is 22-30 ℃, the current is 1-100A, preferably 8-30A, and the time is 60-100 min.
In the process of plating, research personnel not only devote on the researches on the stability of plating solution, the environmental protection of materials, the oxidation resistance of the plating layer and the like, but also have to ensure that whiskers are not easy to grow on a tinned product due to the particularity of the inductance of the magnetic core, thereby avoiding short circuit; the tin plating system selects a C10-C14 alkyl benzyl compound, tin plating is carried out on a nickel plating layer under the action of salt substances, carboxylic acid compounds and the like, only a little Sn-Ni intermetallic compound is generated, particularly when the C10-C14 alkyl benzyl compound is dodecyl dimethyl benzyl ammonium chloride, the wet heat storage reaches 330 days, the surface of the tin plating layer is not slightly convex, the incubation period of whiskers is obviously prolonged, and the quality guarantee period of products is longer. The system belongs to low-foam environment-friendly tin plating liquid, and is convenient for cleaning after plating products.
The invention provides a preparation method of a tin plating solution for magnetic core inductance electroplating, which comprises the following steps:
(1) adding hydroxyl carboxylate, salt substances and polycarboxylic acid into deionized water, and stirring for dissolving;
(2) adding stannous ion source and stirring evenly;
(3) adding C10-C14 alkyl compound.
Compared with the prior art, the invention has the following beneficial effects:
(1) the used materials are mostly food-grade materials or environment-friendly materials, so that the harm to a human body is low, the environmental pollution is less, and the operation of workers does not need to be strictly protected;
(2) the coating of the tin plating liquid of the system has white and bright appearance and excellent tin soldering performance;
(3) the system belongs to low-foam environment-friendly tin plating solution, is convenient for cleaning after plating of products, and has longer quality guarantee period.
Drawings
FIG. 1: EDS chart of plated piece obtained in example 3;
FIG. 2: SEM image of the plating layer of the plated article obtained in example 1;
FIG. 3: SEM image of the plating layer of the plated article obtained in example 2;
FIG. 4: SEM image of the plating layer of the plated article obtained in example 3.
Detailed Description
Example 1: a tin plating solution for magnetic core inductor electroplating, comprising:
(1) hydroxycarboxylic acid salt with mass concentration of 100 g/L;
(2) two kinds of polycarboxylic acid with the mass concentration of 18 g/L;
(3) a stannous ion source with mass concentration of 15 g/L;
(4) a salt substance with a mass concentration of 50 g/L;
(5) a C10-C14 alkyl compound with the mass concentration of 5 g/L;
the hydroxyl carboxylate is sodium gluconate;
the two polycarboxylic acids are tartaric acid and citric acid, and the mass concentration ratio is 1: 1;
the stannous ion source is stannous methanesulfonate;
the salt substance is sodium methanesulfonate;
the C10-C14 alkyl compound is dodecyl dimethyl benzyl ammonium chloride (CAS number: 8001-54-5);
the electroplating conditions of the tin plating solution are as follows: the temperature is 25 ℃, the current is 15A, and the time is 80 min.
A preparation method of tin plating solution for electroplating magnetic core inductance comprises the following steps:
(1) adding hydroxyl carboxylate, salt substances and polycarboxylic acid into deionized water, and stirring for dissolving;
(2) adding stannous ion source and stirring evenly;
(3) adding C10-C14 alkyl compound.
Example 2: a tin plating solution for magnetic core inductor electroplating, comprising:
(1) a hydroxycarboxylic acid salt having a mass concentration of 50 g/L;
(2) two kinds of polycarboxylic acid with the mass concentration of 9 g/L;
(3) a stannous ion source with mass concentration of 5 g/L;
(4) a salt substance with a mass concentration of 30 g/L;
(5) a C10-C14 alkyl compound with the mass concentration of 1 g/L;
the hydroxyl carboxylate is sodium gluconate;
the two polycarboxylic acids are tartaric acid and citric acid, and the mass concentration ratio is 1: 1;
the stannous ion source is stannous methanesulfonate;
the salt substance is sodium methanesulfonate;
the C10-C14 alkyl compound is dodecyl dimethyl benzyl ammonium chloride;
the electroplating conditions of the tin plating solution are as follows: the temperature is 25 ℃, the current is 15A, and the time is 80 min.
A preparation method of tin plating solution for electroplating magnetic core inductance comprises the following steps:
(1) adding hydroxyl carboxylate, salt substances and polycarboxylic acid into deionized water, and stirring for dissolving;
(2) adding stannous ion source and stirring evenly;
(3) adding C10-C14 alkyl compound.
Example 3: a tin plating solution for magnetic core inductor electroplating, comprising:
(1) a hydroxycarboxylic acid salt having a mass concentration of 75 g/L;
(2) two kinds of polycarboxylic acid with the mass concentration of 13.5 g/L;
(3) a stannous ion source with a mass concentration of 10 g/L;
(4) a salt substance with a mass concentration of 45 g/L;
(5) a C10-C14 alkyl compound with the mass concentration of 3 g/L;
the hydroxyl carboxylate is sodium gluconate;
the two polycarboxylic acids are tartaric acid and citric acid, and the mass concentration ratio is 1: 1;
the stannous ion source is stannous methanesulfonate;
the salt substance is sodium methanesulfonate;
the C10-C14 alkyl compound is dodecyl dimethyl benzyl ammonium chloride;
the electroplating conditions of the tin plating solution are as follows: the temperature is 25 ℃, the current is 15A, and the time is 80 min.
A preparation method of tin plating solution for electroplating magnetic core inductance comprises the following steps:
(1) adding hydroxyl carboxylate, salt substances and polycarboxylic acid into deionized water, and stirring for dissolving;
(2) adding stannous ion source and stirring evenly;
(3) adding C10-C14 alkyl compound.
Comparative example 1: tin plating solution for magnetic core inductance electroplating
The difference from example 3 is that, tartaric acid was replaced with gluconic acid,
a method for preparing tin plating solution for electroplating magnetic core inductor, which is the same as that in example 3.
Comparative example 2: tin plating solution for magnetic core inductance electroplating
The difference from example 3 is that citric acid was replaced with gluconic acid.
A method for preparing tin plating solution for electroplating magnetic core inductor, which is the same as that in example 3.
Comparative example 3: tin plating solution for magnetic core inductance electroplating
The difference from example 3 is that the plating temperature was 45 ℃.
A method for preparing tin plating solution for electroplating magnetic core inductor, which is the same as that in example 3.
Comparative example 4: tin plating solution for magnetic core inductance electroplating
The difference from example 3 is that the C10-C14 alkyl compound is dodecyltrimethylammonium chloride (CAS number: 112-00-5).
A method for preparing tin plating solution for electroplating magnetic core inductor, which is the same as that in example 3.
Comparative example 5: tin plating solution for magnetic core inductance electroplating
The difference from example 3 is that the C10-C14 alkyl compound is sodium dodecylbenzenesulfonate (CAS number: 25155-30-0).
A method for preparing tin plating solution for electroplating magnetic core inductor, which is the same as that in example 3.
And (3) performance testing:
1. and (4) EDS detection: EDS detection of the plated article obtained in example 3 revealed that the Sn content was 91.93%, the purity was high, and the impurity contents of Ni and Fe were low (FIG. 1).
2. Coating microstructure: whether the crystals of the plating layer are fine and uniform is observed by SEM.
The plating of the plated part obtained in example 1 is fine and uniform (FIG. 2); the coating obtained in example 2 is fine and uniform (fig. 3); the coating obtained in example 3 was fine and uniform (FIG. 4); the plating layers obtained in comparative examples 1, 2 and 5 are fine and uniform; the plating layers obtained in comparative examples 3 and 4 were rough.
3. Stability of plating solution: during the plating, it was observed whether the tin plating solution was turbid in 65 days.
The plated articles obtained in examples 1 to 3 were not cloudy for 65 days; the plated articles obtained in comparative examples 1 to 3 were cloudy after 65 days; the plated articles obtained in comparative examples 4 and 5 were not cloudy for 65 days.
4. And (3) testing water vapor: the plated articles obtained in examples and comparative examples were placed in a water vapor atmosphere, and it was observed and recorded whether or not the plating layer was changed after 16 hours.
The plating layers of the plated articles obtained in examples 1 to 3 were unchanged; the plated layers of the plated articles obtained in comparative examples 1 to 5 were discolored.
5. Moist heat storage time: the plated articles obtained in examples and comparative examples were left at 55 ℃ and 85% RH for 330 days, and the plated layers were observed by SEM.
The tin-plated surfaces of the plated articles obtained in examples 1 to 3 did not show any hillock or whisker; the tin-plated surfaces of the plated articles obtained in comparative examples 1 to 5 exhibited micro-protrusions or whiskers.
Claims (10)
1. The tin plating solution for electroplating the magnetic core inductor is characterized by comprising the following components:
(1) at least one salt of a hydroxycarboxylic acid;
(2) at least two polycarboxylic acids;
(3) at least one stannous ion source;
(4) at least one salt-like substance, wherein the anion of the salt-like substance is the same as the anion of the stannous ion source;
(5) at least one C10-C14 alkyl compound.
2. The tin plating solution for magnetic core inductor electroplating according to claim 1, wherein the salt of hydroxycarboxylic acid is different from the carboxylate ion of the polycarboxylic acid, and the number of hydroxyl groups of the salt of hydroxycarboxylic acid is equal to or greater than the number of hydroxyl groups of the polycarboxylic acid.
3. The tin plating solution for magnetic core inductor electroplating according to claim 1, wherein the salt of hydroxycarboxylic acid is selected from at least one of sodium gluconate, sodium citrate, sodium tartrate and sodium malate.
4. The tin plating solution for magnetic core inductor electroplating according to claim 1, wherein the polycarboxylic acid is selected from at least two of gluconic acid, citric acid, tartaric acid, and malic acid.
5. The tin plating solution for magnetic core inductor electroplating according to claim 1, wherein the salt of hydroxycarboxylic acid is sodium gluconate, the first polycarboxylic acid is gluconic acid, and the second polycarboxylic acid is citric acid; or the hydroxyl carboxylate is sodium gluconate, the first polycarboxylic acid is tartaric acid, and the second polycarboxylic acid is gluconic acid; or the hydroxyl carboxylate is sodium gluconate, the first polycarboxylic acid is tartaric acid, and the second polycarboxylic acid is citric acid.
6. The tin plating solution for magnetic core inductor electroplating according to claim 1, wherein the mass concentration of the hydroxycarboxylic acid salt is 50-100 g/L.
7. The tin plating solution for magnetic core inductance electroplating according to claim 1, wherein the mass concentration of the polycarboxylic acid is 9-18 g/L.
8. The tin plating solution for magnetic core inductance electroplating according to claim 1, wherein the pH of the tin plating solution is 3 to 5.
9. The tin plating solution for electroplating the magnetic core inductor according to claim 1, wherein the electroplating conditions of the tin plating solution are as follows: the temperature is 22-30 ℃, the current is 1-100A, and the time is 60-100 min.
10. The method for preparing the tin plating solution for the inductance electroplating of the magnetic core according to any one of claims 1 to 9, characterized by comprising the following steps:
(1) adding hydroxyl carboxylate, salt substances and polycarboxylic acid into deionized water, and stirring for dissolving;
(2) adding stannous ion source and stirring evenly;
(3) adding C10-C14 alkyl compound.
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