CN105420795A - Nickel seal electroplating method - Google Patents
Nickel seal electroplating method Download PDFInfo
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- CN105420795A CN105420795A CN201510836850.XA CN201510836850A CN105420795A CN 105420795 A CN105420795 A CN 105420795A CN 201510836850 A CN201510836850 A CN 201510836850A CN 105420795 A CN105420795 A CN 105420795A
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- nickel
- solution
- plating
- complex
- envelope
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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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- 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
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
- C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
- C25D3/16—Acetylenic compounds
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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 nickel seal electroplating method. The nickel seal electroplating method is characterized by comprising Ba complex preparing, nickel seal plating solution preparing and the electroplating process, wherein, a BA complex solution is dropwise added in a bright nickel plating solution firstly, and a nickel seal coating is prepared after a barium sulfate composite nickel plating solution is prepared. The method comprises the specific steps that a, a Ba2+solution and a citrate ion solution are put in a reactor to have a matching reaction, PH is adjusted through a NaOH solution, and the stable Ba complex is formed by Ba2+ and citrate ions under strong stirring; b, under strong stirring, the obtained Ba complex solution is dropwise added in bright electroplated nickel, BaSO4 non-conducting particles are generated through the reaction between Ba2+ released by the Ba complex and SO42- in the plating solution, and the nickel seal plating solution is prepared; and c, the nickel seal plating solution is continuously stirred for 3-10 min, the BaSO4 particles are evenly scattered, and electroplating applying can be started. The method is suitable for the multi-layer nickel micropore chromium technology, the number of micropores of a chromium coating is high, the size is consistent, distribution is even, and the corrosion resistance of the combined coating can be effectively improved.
Description
Technical field
The invention belongs to field of metal surface treatment technology, is a kind of nickel envelope electro-plating method being applicable to multiple layer nickel plating chromium plating.
Background technology
The hole of common layers of chrome or tiny crack lack greatly, and under corrosive medium effect, the nickel that hole and cracks expose and chromium form very active corrosion cell, and wherein nickel dam is anode, and layers of chrome is negative electrode.Because micropore is considerably less, corrosion current concentrates on micropore place, and micropore current density is large, makes corrosion from longitudinally carrying out fast.In bright nickel plating solution, add non-conductive solia particle and nickel codeposition forms composite deposite, on this composite deposite during chromium plating, chromium can not deposit on particulate, thus is formed with the microporous chromium coatings of the micro-pore that is evenly distributed in a large number.When there is corrosion, the corrosion current of the micropore dispersion on surface, makes corrosion laterally carry out, improves the barrier propterty of combined plating.
Nickel envelope particulate mainly some nano level Al conventional at present
2o
3powder, Al
2o
3emulsion, SiO
2powder etc., it is good that nano level particulate has suspension property in the plating solution, is evenly distributed, and complex part each micropore such as to be evenly distributed at the advantage, but also there is certain defect.Nano material is expensive; Nano-particles size is little, specific surface energy is large, thermodynamic instability, in Synthesis and applications process, easily particle agglomeration occurs.Special in electroplate liquid, because electrolyte concentration is high, the electrostatic double layer of nano-particle surface is compressed, and make nanoparticle be more prone to reunite, often need to add polymer organic dispersing agent, thus it is complicated that plating solution is formed, and strengthens plating solution maintenance difficulty.
Summary of the invention
A kind of cost that object of the present invention is exactly deficiency in order to solve prior art and provides is low, the nickel envelope electro-plating method that technique is simple, micropore is evenly distributed, number cells is high.
The present invention adopts following technical solution to realize above-mentioned purpose: a kind of nickel envelope electro-plating method, it is characterized in that, it comprises the preparation of Ba title complex, the preparation of nickel envelope plating solution and electroplating process, first in bright nickel plating solution, drip Ba complex solution, prepare barium sulfate composite nickel-plating solution and prepare nickel envelope coating again, its concrete steps comprise:
A, by Ba
2+solution and citrate ion solution are placed in reactor and complex reaction occur, and regulate PH, under vigorous stirring Ba by NaOH solution
2+stable Ba title complex is formed with lemon acid ion;
B, strongly mix the lower Ba complex solution by gained be added drop-wise to bright nickel plating in, Ba title complex release Ba
2+with SO in plating solution
4 2-reaction generates BaSO
4non-conductive particulate, obtained nickel envelope plating solution;
C, nickel is sealed plating solution Keep agitation 3-10min, make BaSO
4microparticulate is even, can start plating.
Further illustrating as such scheme, in step a process, barium salt concentration range 1 × 10
-4-1 × 10
-2mol/L, citrate ion concentration range 0-0.4mol/L, utilize NaOH solution to regulate PH to be 3-9, Keep agitation 5-30min.
In step a process, the SO in the bright nickel plating solution of gained Ba title complex and step b
4 2-the raw BaSO of reaction
4precipitation and citrate ion, BaSO
4particulate and nickel ion generation codeposition obtain nickel-barium sulfate composite deposite (nickel sealing); Citrate ion coordinates with nickel ion in plating solution and forms title complex, can not pollute plating solution, on Deposit appearance without impact.
In described step a, Ba
2+solution is soluble barium salt, as bariumchloride, nitrate of baryta, barium sulphide, organic barium, coordination agent be can with the coordination agent of barium ion generation complex reaction, as citrate ion, EDTA, polycarboxylate ion; What regulate the pH value of complex solution to adopt is basic solution, except electropositive basic solution aobvious in bright nickel plating solution, as quadrol, and raw NH in the plating solution
4 +, on binding force of cladding material can be made in coating to be deteriorated, fragility increase.
In described step b, bright nickel plating solution is primarily of watt nickel plating bath and bright nickel additive composition; Wherein watt nickel plating bath comprises:
Bright nickel additive comprises:
Above form only lists conventional several bright nickel additives, also has numerous species just not list one by one, as long as the brightening agent that can obtain good bright nickel coating is all applicable to this work technique.
In described step c, electroplating technology flow process comprises: polishing → cleaning → oil removing → cleaning → diluted acid activation → cleaning → bright nickel plating → nickel envelope (composite nickel-plating) → cleaning → chromium plating → cleaning → oven dry.
The beneficial effect that the present invention adopts above-mentioned technical solution to reach is:
Nickel envelope electroplating technology of the present invention is adapted to MULTI-LAYER NICKEL micropore chromium process, and chromium coating number cells is high, in the same size, is evenly distributed, and effectively can improve the corrosion resistance nature of combined plating; Also can be used for common bright nickel technique (composite plating) simultaneously, improve the hardness, wear resistance, solidity to corrosion etc. of coating; Do not need to add the more expensive particulate such as aluminum oxide, titanium oxide, silicon oxide of price, cost is very low.
Accompanying drawing explanation
Fig. 1 is the metallurgical microscopic of chromium coating after acid copper-plating of the present invention;
Fig. 2 is the SEM figure of nickel of the present invention envelope coating;
Fig. 3 a is the white point EDS spectrum of Fig. 2;
Fig. 3 b is the non-white point EDS spectrum of Fig. 2;
Fig. 4 is the metallurgical microscopic of chromium coating after acid copper-plating of the present invention;
Fig. 5 is the SEM figure of nickel of the present invention envelope coating;
Fig. 6 a is the white point EDS spectrum of Fig. 4;
Fig. 6 b is the non-white point EDS spectrum of Fig. 4;
Fig. 7 is the metallurgical microscopic of chromium coating after acid copper-plating of the present invention;
Fig. 8 is the SEM figure of nickel of the present invention envelope coating;
Fig. 9 a is the white point EDS spectrum of Fig. 7;
Fig. 9 b is the non-white point EDS spectrum of Fig. 7.
Embodiment
The present invention is a kind of nickel envelope electro-plating method, and it comprises the preparation of Ba title complex, the preparation of nickel envelope plating solution and electroplating process, first in bright nickel plating solution, drips Ba complex solution, and prepare barium sulfate composite nickel-plating solution and prepare nickel envelope coating again, its concrete steps comprise:
A, by Ba
2+solution and citrate ion solution are placed in reactor and complex reaction occur, and regulate PH, under vigorous stirring Ba by NaOH solution
2+stable Ba title complex is formed with lemon acid ion;
B, strongly mix the lower Ba complex solution by gained be added drop-wise to bright nickel plating in, Ba title complex release Ba
2+with SO in plating solution
4 2-reaction generates BaSO
4non-conductive particulate, obtained nickel envelope plating solution;
C, nickel is sealed plating solution Keep agitation 3-10min, make BaSO
4microparticulate is even, can start plating.
Further, in step a process, barium salt concentration range 1 × 10
-4-1 × 10
-2mol/L, citrate ion concentration range 0-0.4mol/L, utilize NaOH solution to regulate PH to be 3-9, Keep agitation 5-30min.SO in the bright nickel plating solution of gained Ba title complex and step b
4 2-the raw BaSO of reaction
4precipitation and citrate ion, BaSO
4particulate and nickel ion generation codeposition obtain nickel-barium sulfate composite deposite; Citrate ion coordinates with nickel ion in plating solution and forms title complex, can not pollute plating solution, on Deposit appearance without impact.
In described step a, Ba
2+solution is soluble barium salt, as bariumchloride, nitrate of baryta, barium sulphide, organic barium, coordination agent be can with the coordination agent of barium ion generation complex reaction, as citrate ion, EDTA, polycarboxylate ion; What regulate the pH value of complex solution to adopt is basic solution, except electropositive basic solution aobvious in bright nickel plating solution, as quadrol, and raw NH in the plating solution
4 +, on binding force of cladding material can be made in coating to be deteriorated, fragility increase.
In described step b, bright nickel plating solution is primarily of watt nickel plating bath and bright nickel additive composition; Wherein watt nickel plating bath comprises:
Bright nickel additive comprises:
Above form only lists conventional several bright nickel additives, also has numerous species just not list one by one, as long as the brightening agent that can obtain good bright nickel coating is all applicable to this work technique.
Further, after described step c, measure pore density by acid copper-plating method.
Further, in described step c, electroplating technology flow process comprises: polishing → cleaning → oil removing → cleaning → diluted acid activation → cleaning → bright nickel plating → nickel envelope (composite nickel-plating) → cleaning → chromium plating → cleaning → oven dry.Wherein, oil removal process be adopt electrochemical deoiling, formula and processing condition as follows:
In oil removing and after workpiece is washed, the diluted acid activation procedure carried out, its activation solution adopted is the dilute hydrochloric acid of 10%;
After diluted acid activation, through workpiece washing, then carry out Bright Nickel Electroplating operation, Bright Nickel Electroplating recipe optimization:
Nickel envelope electroplating work procedure is carried out, the preparation of nickel envelope electroplate liquid and technique after Bright Nickel Electroplating:
1. by described formulated bright nickel plating solution;
2. be 1 × 10 by preparing concentration in step a
-4~ 1 × 10
-2the Ba complex solution of mol/L;
3. under vigorous stirring, the Ba complex solution prepared is added in bright nickel plating solution, forms BaSO rapidly
4particulate, Keep agitation 5min, makes microparticulate even;
4. the workpiece having plated bright nickel does not need washing, directly chargedly enters nickel sealing groove, according to cathode current density 4A/dm
2carry out plating 2min;
Workpiece through nickel envelope operation carries out electrodeposited chromium operation, electrodeposited chromium recipe optimization after washing:
After workpiece washing, adopt acid copper-plating to measure the pore density of chromium coating, concrete recipe optimization is as follows:
After workpiece acid coppering, count out with metaloscope amplifying observation, the copper that calculates unit surface of taking pictures and be nickel envelope micropore number.
Through above-mentioned technical process, the pore density of chromium coating can reach 0.8 × 10
4~ 2 × 10
5individual/cm
2, micropore is evenly distributed, in the same size, can significantly improve the corrosion resistance nature of MULTI-LAYER NICKEL chromium plating combined plating.Ba title complex and SO
4 2-the BaSO that reaction generates
4during as nickel envelope additive, BaSO
4microparticle surfaces has adsorbed one deck coordination agent, can stop to a certain extent between particle on the one hand and reunite, improve particulate dispersed in the plating solution; On the other hand coordination agent can further with Ni
2+coordinate, strengthen the positive polarity of particulate, promote itself and the codeposition of nickel ion, increase compounding quantity, thus the pore density of raising chromium coating.Therefore, compared with sealing additive with other nickel, (as aluminum oxide, silicon-dioxide, titanium dioxide) is compared and is had that add-on is few, number cells advantages of higher.
Below in conjunction with specific embodiment, the technical program is explained in detail.
Embodiment 1
Preparation 100mlBa title complex and 250ml nickel envelope plating solution, carry out according to following operational condition.
Ba complex solution composition and processing condition:
| Composition | Concentration |
| Bariumchloride BaCl 2.2H 2O | 8.2×10 -3mol/L |
| Trisodium citrate C 6H 5Na 3O 7.2H 2O | 1.7×10 -2mol/L |
| PH | 7.4 |
Nickel envelope plating solution composition and processing condition:
Workpiece carries out: oil removing, activation, Bright Nickel Electroplating, and electronickelling is sealed, electroplated decorative chromium, then presses acid copper-plating method mensuration chromium coating pore density, and number cells can reach 3.1 × 10
4individual/cm
2.After acid copper-plating, the metallurgical microscopic of chromium coating and nickel sealing SEM are shown in Fig. 1 and Fig. 2 respectively.
Embodiment 2
Preparation 100mlBa title complex and 250ml nickel envelope plating solution, carry out according to following operational condition.
Ba complex solution composition and processing condition:
| Composition | Concentration |
| Bariumchloride BaCl 2.2H 2O | 1.6×10 -3mol/L |
| Trisodium citrate C 6H 5Na 3O 7.2H 2O | 6.8×10 -2mol/L |
| PH | 7.5 |
Nickel envelope plating solution composition and processing condition: with embodiment 1.
Workpiece carries out: oil removing, activation, Bright Nickel Electroplating, and electronickelling is sealed, electroplated decorative chromium, then presses acid copper-plating method mensuration chromium coating pore density, and number cells can reach 5.1 × 10
4individual/cm
2.After acid copper-plating, the metallurgical microscopic of chromium coating and nickel sealing SEM are shown in Fig. 4 and Fig. 5 respectively.
Embodiment 3
Preparation 100mlBa title complex and 250ml nickel envelope plating solution, carry out according to following operational condition.
Ba complex solution composition and processing condition:
| Composition | Concentration |
| Bariumchloride BaCl 2.2H 2O | 3.4×10 -3mol/L |
| Trisodium citrate C 6H 5Na 3O 7.2H 2O | 1.4×10 -2mol/L |
| PH | 7.5 |
Nickel envelope plating solution composition and processing condition: with embodiment 1.
Workpiece carries out: oil removing, activation, Bright Nickel Electroplating, and electronickelling is sealed, electroplated decorative chromium, then presses acid copper-plating method mensuration chromium coating pore density, and number cells can reach 8.9 × 10
4individual/cm
2.After acid copper-plating, the metallurgical microscopic of chromium coating and nickel sealing SEM are shown in Fig. 7 and Fig. 8 respectively.
Nickel envelope additive of the present invention, can arrange in pairs or groups with silicon-dioxide and use.Add the effect that silicon-dioxide mainly plays two aspects, (1) viscosity of plating solution can be made to increase, increase the suspension property of nickel envelope particulate, delayed fallout speed, thus nickel envelope particulate is more evenly distributed in the plating solution, ensure that particulate fully contacts with each position of plating piece, reduce the micropore gap of each of plating piece; (2) can be used as the dispersion agent of nickel envelope particulate, reduce the probability of collision between nickel envelope particulate, prevent the reunion between particle to a certain extent, increase the stability of nickel sealing liquid.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (7)
1. a nickel envelope electro-plating method, it is characterized in that, it comprises the preparation of Ba title complex, the preparation of nickel envelope plating solution and electroplating process, first in bright nickel plating solution, drips Ba complex solution, prepare barium sulfate composite nickel-plating solution and prepare nickel envelope coating again, its concrete steps comprise:
A, by Ba
2+solution and citrate ion solution are placed in reactor and complex reaction occur, and regulate PH, under vigorous stirring Ba by NaOH solution
2+stable Ba title complex is formed with lemon acid ion;
B, strongly mix the lower Ba complex solution by gained be added drop-wise to bright nickel plating in, Ba title complex release Ba
2+with SO in plating solution
4 2-reaction generates BaSO
4non-conductive particulate, obtained nickel envelope plating solution;
C, nickel is sealed plating solution Keep agitation 3-10min, make BaSO
4microparticulate is even, can start plating.
2. nickel envelope electro-plating method according to claim 1, is characterized in that, in step a process, and barium salt concentration range 1 × 10
-4-1 × 10
-2mol/L, citrate ion concentration range 0-0.4mol/L, utilize NaOH solution to regulate PH to be 3-9, Keep agitation 5-30min; SO in the bright nickel plating solution of gained Ba title complex and step b
4 2-the raw BaSO of reaction
4precipitation and citrate ion, BaSO
4particulate and nickel ion generation codeposition obtain nickel-barium sulfate composite deposite; Citrate ion coordinates with nickel ion in plating solution and forms title complex.
3. nickel envelope electro-plating method according to claim 1, is characterized in that, in described step a, and Ba
2+solution is soluble barium salt; Coordination agent be can with the coordination agent of barium ion generation complex reaction; What regulate the pH value of complex solution to adopt is basic solution.
4. nickel envelope electro-plating method according to claim 1, it is characterized in that, in described step b, bright nickel plating solution comprises watt nickel plating bath and bright nickel additive.
5. nickel envelope electro-plating method according to claim 4, it is characterized in that, watt nickel plating bath comprises:
6. nickel envelope electro-plating method according to claim 4, it is characterized in that, bright nickel additive comprises:
7. nickel envelope electro-plating method according to claim 1, it is characterized in that, in described step c, electroplating technology flow process comprises: polishing → cleaning → oil removing → cleaning → diluted acid activation → cleaning → bright nickel plating → nickel envelope → cleaning → chromium plating → cleaning → oven dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510836850.XA CN105420795A (en) | 2015-11-25 | 2015-11-25 | Nickel seal electroplating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510836850.XA CN105420795A (en) | 2015-11-25 | 2015-11-25 | Nickel seal electroplating method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105420795A true CN105420795A (en) | 2016-03-23 |
Family
ID=55499321
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510836850.XA Pending CN105420795A (en) | 2015-11-25 | 2015-11-25 | Nickel seal electroplating method |
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| Country | Link |
|---|---|
| CN (1) | CN105420795A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3644183A (en) * | 1963-01-09 | 1972-02-22 | Res Holland Nv | Process for coating an object with a bright nickel/chromium coatin |
| CN1398789A (en) * | 2002-08-13 | 2003-02-26 | 华北工学院 | Prepn of nano barium sulfate |
| CN102766889A (en) * | 2012-08-20 | 2012-11-07 | 深圳市天泽科技实业有限公司 | Nickel sealing and plating solution and nickel sealing plating process |
| CN103626219A (en) * | 2013-12-19 | 2014-03-12 | 贵州红星发展股份有限公司 | Nano barium sulfate and preparation method thereof |
-
2015
- 2015-11-25 CN CN201510836850.XA patent/CN105420795A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3644183A (en) * | 1963-01-09 | 1972-02-22 | Res Holland Nv | Process for coating an object with a bright nickel/chromium coatin |
| CN1398789A (en) * | 2002-08-13 | 2003-02-26 | 华北工学院 | Prepn of nano barium sulfate |
| CN102766889A (en) * | 2012-08-20 | 2012-11-07 | 深圳市天泽科技实业有限公司 | Nickel sealing and plating solution and nickel sealing plating process |
| CN103626219A (en) * | 2013-12-19 | 2014-03-12 | 贵州红星发展股份有限公司 | Nano barium sulfate and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 何湘柱 等: "镍封新工艺一复合电镀镍-硫酸钡", 《电镀与涂饰》 * |
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Inventor after: Zong Gaoliang Inventor after: He Xiangzhu Inventor after: Xie Jinping Inventor after: Qin Hua Inventor before: Zong Gaoliang Inventor before: Qin Hua Inventor before: Xie Jinping Inventor before: He Xiangzhu |
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Effective date of registration: 20161215 Address after: Dali Town, Nanhai District Changhong Ling Industrial Zone 528200 Guangdong city of Foshan Province Applicant after: Guangdong Zhizhuo Precision Metal Technology Co., Ltd. Applicant after: Guangdong University of Technology Address before: Dali Town, Nanhai District Changhong Ling Industrial Zone 528200 Guangdong city of Foshan Province Applicant before: Guangdong Zhizhuo Precision Metal Technology Co., Ltd. |
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