CN111575750B - Cyanide-free electroplating nano-silver additive - Google Patents
Cyanide-free electroplating nano-silver additive Download PDFInfo
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- CN111575750B CN111575750B CN202010666465.6A CN202010666465A CN111575750B CN 111575750 B CN111575750 B CN 111575750B CN 202010666465 A CN202010666465 A CN 202010666465A CN 111575750 B CN111575750 B CN 111575750B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000000654 additive Substances 0.000 title claims abstract description 34
- 230000000996 additive effect Effects 0.000 title claims abstract description 33
- 238000009713 electroplating Methods 0.000 title claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000000080 wetting agent Substances 0.000 claims abstract description 9
- 238000005282 brightening Methods 0.000 claims abstract description 8
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003223 protective agent Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- JNMRHUJNCSQMMB-UHFFFAOYSA-N sulfathiazole Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CS1 JNMRHUJNCSQMMB-UHFFFAOYSA-N 0.000 claims description 12
- 229960001544 sulfathiazole Drugs 0.000 claims description 12
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 12
- RAABOESOVLLHRU-UHFFFAOYSA-N diazene Chemical compound N=N RAABOESOVLLHRU-UHFFFAOYSA-N 0.000 claims description 8
- 229910000071 diazene Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- AERRGWRSYANDQB-UHFFFAOYSA-N azanium;dodecane-1-sulfonate Chemical compound [NH4+].CCCCCCCCCCCCS([O-])(=O)=O AERRGWRSYANDQB-UHFFFAOYSA-N 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- MVCZKPMTGFFULA-UHFFFAOYSA-N n-pyrimidin-4-ylacetamide Chemical compound CC(=O)NC1=CC=NC=N1 MVCZKPMTGFFULA-UHFFFAOYSA-N 0.000 claims description 6
- 229920001083 polybutene Polymers 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- SEEPANYCNGTZFQ-UHFFFAOYSA-N sulfadiazine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CC=N1 SEEPANYCNGTZFQ-UHFFFAOYSA-N 0.000 claims description 6
- 229960004306 sulfadiazine Drugs 0.000 claims description 6
- 150000005005 aminopyrimidines Chemical class 0.000 claims description 4
- -1 propane pyridinium sulfonate Chemical compound 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- GOUILHYTHSOMQJ-UHFFFAOYSA-N gamma-butenolide Natural products CCC1OC(=O)C=C1 GOUILHYTHSOMQJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229920001748 polybutylene Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- VIESAWGOYVNHLV-UHFFFAOYSA-N 1,3-dihydropyrrol-2-one Chemical compound O=C1CC=CN1 VIESAWGOYVNHLV-UHFFFAOYSA-N 0.000 abstract 1
- ZPOODPZCZLCUAN-UHFFFAOYSA-N 3,4-dihydro-1h-pyridin-2-one Chemical compound O=C1CCC=CN1 ZPOODPZCZLCUAN-UHFFFAOYSA-N 0.000 abstract 1
- 239000011247 coating layer Substances 0.000 abstract 1
- 238000002845 discoloration Methods 0.000 abstract 1
- 230000007774 longterm Effects 0.000 abstract 1
- 238000007747 plating Methods 0.000 description 34
- 229910052709 silver Inorganic materials 0.000 description 24
- 239000004332 silver Substances 0.000 description 24
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- UFULAYFCSOUIOV-UHFFFAOYSA-N cysteamine Chemical compound NCCS UFULAYFCSOUIOV-UHFFFAOYSA-N 0.000 description 4
- 229960003151 mercaptamine Drugs 0.000 description 4
- XSUMSESCSPMNPN-UHFFFAOYSA-N propane-1-sulfonate;pyridin-1-ium Chemical compound C1=CC=NC=C1.CCCS(O)(=O)=O XSUMSESCSPMNPN-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- ZKPTZRGIFZZOFZ-UHFFFAOYSA-N 5-[2-[3-(aminomethyl)anilino]pyrimidin-4-yl]-n-ethyl-4-methyl-1,3-thiazol-2-amine Chemical compound S1C(NCC)=NC(C)=C1C1=CC=NC(NC=2C=C(CN)C=CC=2)=N1 ZKPTZRGIFZZOFZ-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000003949 imides Chemical class 0.000 description 2
- 150000003951 lactams Chemical class 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000005494 tarnishing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- LFAGQMCIGQNPJG-UHFFFAOYSA-N silver cyanide Chemical compound [Ag+].N#[C-] LFAGQMCIGQNPJG-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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
- C25D3/46—Electroplating: Baths therefor from solutions of silver
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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
本发明一种无氰电镀纳米银添加剂中分别含主光亮剂60~80g/L、辅助光亮剂10~20g/L、表面润湿剂5~10g/L和保护剂1~3g/L，其中主光亮剂由25%~50%的γ‑丁烯内酰胺、10%~15%的聚丁烯二酰亚胺、15%~35%的δ‑戊烯内酰胺、10%~15%的聚戊烯二酰亚胺和10%~15%的邻苯二甲酰亚胺组成。本发明添加剂能有效提高镀层光亮度及耐变色能力，在室温下即可达到高光亮与晶粒细化效果，镀层光亮度可达600Gu以上，晶粒可细化至纳米级；稳定性强，在长时间电镀作业或静置后仍能起到优秀的光亮效果；且生产成本低，效率高，绿色环保。
The nano-silver additive for cyanide-free electroplating of the present invention contains 60-80 g/L of main brightener, 10-20 g/L of auxiliary brightening agent, 5-10 g/L of surface wetting agent and 1-3 g/L of protective agent, respectively. The main brightener is composed of 25%~50% γ-butenolactam, 10%~15% polybutenedimide, 15%~35% δ-pentenolactam, 10%~15% It is composed of polyglutarimide and 10%~15% phthalimide. The additive of the invention can effectively improve the brightness and discoloration resistance of the coating layer, and can achieve high brightness and grain refinement effects at room temperature. It can still play an excellent bright effect after long-term electroplating operation or standing; and the production cost is low, the efficiency is high, and it is green and environmentally friendly.
Description
Technical Field
The invention relates to a cyanide-free electroplating nano-silver additive, which is an additive used in silver electroplating under direct current or pulse conditions in a cyanide-free plating solution, and particularly belongs to the technical field of electroplating additives.
Background
With the increasing living standard and the development of science and technology, the demand and the requirement of people on silver plating parts are increased day by day. The silver plating layer for industrial production generally adopts an electroplating means, the current mainstream silver electroplating system contains cyanide which is often extremely toxic, and the cyanide electroplating is gradually eliminated along with the enhancement of environmental protection consciousness and safety consciousness. However, it is difficult to obtain a dense and bright plating layer, even if a silver electrodeposition layer is prepared without any additive, regardless of the plating conditions usedDendrite segregation may occur. Therefore, it is very important to develop a stable plating additive capable of effectively improving the plating state. At present, cyanide-free silver electroplating is the development direction of green electroplating, but the problems of poor glossiness, low binding force and the like exist, and cyanide electroplating is still difficult to replace. The cyanide-free bright silver plating solution mentioned in patent CN 107299367A has a current density range of 0.1-0.2A/dm2The current density of the conventional cyanide silver plating is 0.2-1.2A/dm2On the one hand, a lower current density leads to low production efficiency, and on the other hand, a narrower current density interval leads to lower yield. The alkaline cyanide-free silver plating electroplating solution and the silver plating method provided in patent CN 1073130841A have the plating temperature range of 40-60 ℃, and the plating can be carried out only by heating, so that the energy consumption in production is increased, the production cost is improved, and the production efficiency is lower. The cyanide-free bright silver plating bath mentioned in patent CN201710738117.3 gave a silver plating layer with a gloss of only 110 Gu.
Therefore, the additive of the cyanide-free silver electroplating solution, which is stable, efficient and environment-friendly, can improve the displacement capability of the plating solution, the glossiness of a silver coating and the grain refinement degree of the silver coating and widen the current density range of the plating solution at room temperature, is always a research hotspot in the field of cyanide-free silver plating.
Disclosure of Invention
The invention aims to provide a cyanide-free electroplating nano silver additive, which mainly depends on imide or lactam containing unsaturated bonds, can widen the current density range of a plating solution, effectively improve the anti-tarnishing capability and glossiness of a silver deposition layer obtained by electroplating and enable the plating layer to achieve mirror surface brightness.
The cyanide-free electroplating nano-silver additive disclosed by the invention consists of a main brightener 60-80 g/L, an auxiliary brightener 10-20 g/L, a surface wetting agent 5-10 g/L and a surface wetting agent 1-3 g/L;
the main brightening agent consists of 25-50% of gamma-butenolide, 10-15% of polybutene diimide, 15-35% of delta-pentenoic lactam, 10-15% of polypentene diimide and 10-15% of phthalimide in percentage by mass; the auxiliary brightening agent consists of 40-50% of aminopyrimidine, 20-30% of 4-acetamidopyrimidine and 20-30% of sulfadiazine; the protective agent consists of 50-80% of sulfathiazole thioglycolic acid, 10-25% of sulfathiazole monoethanolamine and 10-25% of propane pyridinium sulfonate; the surface wetting agent consists of 30-40% of ammonium dodecyl sulfonate, 30-40% of sodium dodecyl benzene sulfonate and 30-40% of sodium dodecyl sulfate.
The preparation process of the additive comprises the following steps:
adjusting the pH value to 10-11 by using a sodium hydroxide or potassium hydroxide solution in 700 mL of pure water, sequentially adding 5-10 g of a surface wetting agent, 60-80 g of a main light agent and 10-20 g of an auxiliary brightening agent under the condition of fully and uniformly stirring, then adding a mixture of 1-3 g of a protective agent and 150mL of pure water, uniformly mixing, and continuously adding pure water until the volume of the mixture reaches 1L to obtain the cyanide-free electroplating nano-silver additive.
The molecular weight of the polybutylene diimide and the polypentene diimide is less than 2000.
The application conditions of the additive are as follows: the pH range is 7.5-11.5, and the temperature range is 10-55 ℃.
The invention has the beneficial effects that:
1. the cyanide-free electroplating nano silver additive can refine crystal grains of a plating layer and reduce internal stress of the plating layer, and mainly depends on imide or lactam of unsaturated bonds contained in the cyanide-free electroplating nano silver additive, so that the current density range of the plating solution can be widened, the anti-tarnishing capability and the glossiness of a silver deposition layer obtained by electroplating are effectively improved, the mirror surface brightness of the plating layer can be achieved, the maximum glossiness can reach more than 600Gu, the crystal grains of the plating layer can be refined to be nano-scale, and the average size is 30-80 nm.
2. The cyanide-free silver plating additive does not contain harmful cyanide components, is green and environment-friendly, belongs to the development direction of green electroplating, has strong stability, and still has good brightening effect after long-time electroplating operation or long-time standing.
3. The cyanide-free silver plating additive can play an excellent bright effect when being used for electroplating at room temperature, does not need heating in the electroplating process, and has low production cost and high efficiency.
Drawings
FIG. 1 is a diagram of a plated article obtained in a Hull cell without adding a brightener to the silver plating solution of the present invention;
FIG. 2 is a diagram of a plated article obtained in a Hull cell after addition of a cyanide-free silver plating additive in example 1 of the present invention;
FIG. 3 shows the gloss test results of the plated article obtained in a Hull cell after the cyanide-free silver plating additive was added in example 1 of the present invention;
FIG. 4 is an FESEM image of a plated article obtained in a Hell cell after a plating layer is enlarged by 10 ten thousand times after a cyanide-free silver plating additive is added in example 1 of the present invention.
Detailed Description
Example 1
The preparation process of the cyanide-free electroplating nano silver additive comprises the following steps: (1) 700 mL of pure water was added to a 1L container; (2) adding a proper amount of sodium hydroxide solution to adjust the pH value to 10.5; (3) adding 3g of ammonium dodecyl sulfonate, 3g of sodium dodecyl benzene sulfonate and 3g of sodium dodecyl sulfate into the container, stirring and dissolving; (4) adding 35 g of gamma-butenolactam, 15 g of delta-pentenolactam, 10g of phthalimide, 10g of polybutene diimide-1000 and 10g of polypentene diimide-1000 into a container, stirring and dissolving; (5) then 5g of aminopyrimidine, 2 g of 4-acetamidopyrimidine and 3g of sulfadiazine are added into the container, stirred and dissolved; (6) dissolving 1.85g of sulfathiazole thioglycolic acid, 0.3 g of sulfathiazole thioethanolamine and 0.35 g of pyridinium propanesulfonate in 150mL of pure water, pouring into a container, and stirring to uniformly mix; (7) adding pure water to 1L. The cyanide-free electroplating nano silver additive is added into the silver plating solution produced in a certain factory, and a physical diagram obtained in a Hell cell is shown in figure 2. The plating layer can clearly reflect the characters on the book, and the mirror surface brightness is achieved; the gloss test result is shown in figure 3, and the gloss can reach over 600 Gu; the FESEM image of the coating is shown in figure 4, and the average size of the coating crystal grains is 30-80 nm.
Example 2
The preparation process of the cyanide-free electroplating nano silver additive comprises the following steps: (1) 700 mL of pure water was added to a 1L container; (2) adding a proper amount of potassium hydroxide solution to adjust the pH value to 10.8; (3) then adding 3g of ammonium dodecyl sulfonate, 3g of sodium dodecyl benzene sulfonate and 4 g of sodium dodecyl sulfate into the container, stirring and dissolving; (4) adding 35 g of gamma-butenolactam, 15 g of delta-pentenolactam, 10g of phthalimide, 10g of polybutene diimide-1000 and 10g of polypentene diimide-1000 into a container, stirring and dissolving; (5) then 5g of aminopyrimidine, 3g of 4-acetamidopyrimidine and 2 g of sulfadiazine are added into the container, stirred and dissolved; (6) dissolving 1.85g of sulfathiazole thioglycolic acid, 0.35 g of sulfathiazole thioethanolamine and 0.35 g of pyridinium propanesulfonate in 150mL of pure water, pouring into a container, and stirring to uniformly mix; (7) adding pure water to 1L.
Example 3
The preparation process of the cyanide-free electroplating nano silver additive comprises the following steps: (1) 700 mL of pure water was added to a 1L container; (2) adding a proper amount of sodium hydroxide solution to adjust the pH value to 10.5; (3) adding 4 g of ammonium dodecyl sulfonate, 3g of sodium dodecyl benzene sulfonate and 3g of sodium dodecyl sulfate into the container, stirring and dissolving; (4) adding 35 g of gamma-butenolactam, 15 g of delta-pentenolactam, 10g of phthalimide, 10g of polybutene diimide-1000 and 10g of polypentene diimide-1000 into a container, stirring and dissolving; (5) then 5g of aminopyrimidine, 2 g of 4-acetamidopyrimidine and 3g of sulfadiazine are added into the container, stirred and dissolved; (6) dissolving 1.5 g of sulfathiazole thioglycolic acid, 0.35 g of sulfathiazole thioethanolamine and 0.35 g of pyridinium propanesulfonate in 150mL of pure water, pouring into a container, and stirring to uniformly mix; (7) adding pure water to 1L.
Example 4
The preparation process of the cyanide-free electroplating nano silver additive comprises the following steps: (1) 700 mL of pure water was added to a 1L container; (2) adding a proper amount of sodium hydroxide solution to adjust the pH value to 10.8; (3) adding 3g of ammonium dodecyl sulfonate, 4 g of sodium dodecyl benzene sulfonate and 3g of sodium dodecyl sulfate into the container, stirring and dissolving; (4) then 40 g of gamma-butenolactam, 16 g of delta-pentenolactam, 8g of phthalimide, 8g of polybutene diimide-1000 and 8g of polypentene diimide-1000 are added into the container, stirred and dissolved; (5) adding 4 g aminopyrimidine, 3g 4-acetamidopyrimidine and 3g sulfadiazine into the container, stirring and dissolving; (6) dissolving 1.5 g of sulfathiazole thioglycolic acid, 0.35 g of sulfathiazole thioethanolamine and 0.35 g of pyridinium propanesulfonate in 150mL of pure water, pouring into a container, and stirring to uniformly mix; (7) adding pure water to 1L.
The foregoing exemplary embodiments have described the invention in more detail and in greater detail, but are not intended to limit the invention to the details given herein. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. The cyanide-free electroplating nano silver additive is characterized in that: the additive consists of a main brightener, an auxiliary brightener, a protective agent and a surface wetting agent, wherein the additive contains 60-80 g/L of the main brightener, 10-20 g/L of the auxiliary brightener, 5-10 g/L of the surface wetting agent and 1-3 g/L of the protective agent respectively;
the main brightening agent consists of 25-50% of gamma-butenolide, 10-15% of polybutene diimide, 15-35% of delta-pentenoic lactam, 10-15% of polypentene diimide and 10-15% of phthalimide in percentage by mass; the auxiliary brightening agent consists of 40-50% of aminopyrimidine, 20-30% of 4-acetamidopyrimidine and 20-30% of sulfadiazine; the protective agent consists of 50-80% of sulfathiazole thioglycolic acid, 10-25% of sulfathiazole monoethanolamine and 10-25% of propane pyridinium sulfonate; the surface wetting agent consists of 30-40% of ammonium dodecyl sulfonate, 30-40% of sodium dodecyl benzene sulfonate and 30-40% of sodium dodecyl sulfate;
the preparation process of the additive comprises the following steps:
adjusting the pH value to 10-11 by using a sodium hydroxide or potassium hydroxide solution in 700 mL of pure water, sequentially adding 5-10 g of a surface wetting agent, 60-80 g of a main light agent and 10-20 g of an auxiliary brightening agent under the condition of fully and uniformly stirring, then adding a mixture of 1-3 g of a protective agent and 150mL of pure water, uniformly mixing, and continuously adding pure water until the volume of the mixture reaches 1L to obtain a cyanide-free electroplating nano-silver additive;
the molecular weight of the polybutylene diimide and the polypentene diimide is less than 2000.
2. The cyanide-free electroplated nanosilver additive of claim 1, wherein: the application conditions of the additive are as follows: the pH range is 7.5-11.5, and the temperature range is 10-55 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3751021A4 (en) * | 2018-02-08 | 2021-11-10 | Daicel Corporation | Plating film |
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