CN102943290B - Method for electroplating of nickel-cobalt alloy on electronic packaging casing - Google Patents
Method for electroplating of nickel-cobalt alloy on electronic packaging casing Download PDFInfo
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- CN102943290B CN102943290B CN201210486279.XA CN201210486279A CN102943290B CN 102943290 B CN102943290 B CN 102943290B CN 201210486279 A CN201210486279 A CN 201210486279A CN 102943290 B CN102943290 B CN 102943290B
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Abstract
The invention discloses a method for electroplating of a nickel-cobalt alloy on an electronic packaging casing. The method includes the following steps that (1) checking and preparing before plating are conducted; (2) processing before plating is conducted and includes that a surface to be plated is washed; (3) nickel is pre-plated; (4) nickel is plated; (5) the nickel-cobalt alloy is plated: an anode is a sheet nickel, electroplating liquid is composed of 180-220g/L NiSO4-6H2O, 35-45 g/L H3BO3, 10-18 g/L NaCl and 3-8 g/L CoSO4-7H2O3, and the electroplating conditions are that pH is 5-6, current density is 1-2A/dm2, and the temperature is 50-60 DEG C; (6) gold is pre-plated; (7) gold is plated; (8) post-processing is conducted. Samples are plated by using the electroplating liquid and the electroplating conditions, cobalt content in the nickel-cobalt plating can be controlled to be 15%-30% stably, and a requirement that a theoretical analysis value of cobalt content in the plating is larger than or equal to 10.5% can be met.
Description
Technical field
The present invention relates to a kind of method of nickel-cobalt alloy plating, especially a kind of method of electronic encapsulation shell nickel-cobalt alloy plating.
Background technology
Nickel-cobalt alloy plating in industrial application usually used as fancy alloy and magneticalloy.The nickel cobalt (alloy) of cobalt contents less than 30% has white metal outward appearance, and hardness is moderate, has good wear resistance and chemical stability.At present, disclosed Application to Electronic Industry is mainly used in the disk of computer storage system, the surface magnetism coating of magnetic drum at home.From the 90's of 20th century, some countries successively adopt the nickel-cobalt alloy plating of w (Co) 5% ~ 40% to replace nickel coating in ceramic packing.Nickel cobalt (alloy) is diffusion impervious layer more more efficiently than nickel.The present invention has researched and developed a kind of Ni-Co alloy electroplating process, this process application is in the manufacturing of electronic encapsulation shell, using the prime coat of nickel-cobalt alloy plating as electronic encapsulation shell Gold plated Layer, effectively can improve the reliability of electronic encapsulation shell chip high-temperature soldering, and improve its high temperature resistance metachrosis, effectively to avoid by pure nickel as nickel under brittle cracking problem during layer gold prime coat and high temperature to layer gold surface diffusion problem, improve performance and the reliability step of ceramic packing shell.
For electronic encapsulation shell application requiring, cobalt contents in nickel cobalt (alloy) is vital, the present invention is controlled by the preparation of nickel-cobalt alloy plating plating solution, electroplating current density, realizes the control of cobalt contents in nickel-cobalt alloy plating, reaches electronic encapsulation shell application requiring.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of electronic encapsulation shell nickel-cobalt alloy plating, and nickel cobalt coating cobalt contents Absorbable organic halogens is controlled between 15% ~ 30%, can meet the theoretical analysis value requirement of coating cobalt contents >=10.5%.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of electronic encapsulation shell nickel-cobalt alloy plating, comprises the following steps: (1) carries out plating front inspection and preparation before plating; (2) treatment before plating: surface to be plated is cleaned; (3) nickel preplating; (4) nickel plating; (5) nickel plating cobalt: anode is sheet nickel,
Consisting of of electroplate liquid:
NiSO
4·6H
2O 180～220 g/L
H
3BO
335～45g/L
NaCl 10～18g/L
CoSO
4·7H
2O 3～8g/L；
Plating conditions is: pH is 5 ~ 6 current densities is 1 ~ 2A/dm
2temperature is 50 ~ 60 DEG C;
(6) gold-plated in advance; (7) gold-plated; (8) aftertreatment.
The purity of anode electrolysis nickel plate is 99.99%.
CoSO in electroplate liquid
47H
2the optimum content of O is 5g/L.
Optimum current density is 1A/dm
2.
Use electroplate liquid of the present invention and plating conditions to carry out sample plating, its nickel cobalt coating cobalt contents Absorbable organic halogens is controlled between 15% ~ 30%, can meet the theoretical analysis value requirement of the minimum cobalt contents 10.5% of theory that electronic encapsulation shell chip reliably welds.
Electronickelling cobalt liquor adopts single nickel salt and rose vitriol for providing the main salt of two metal ion species, and the advantage of two kinds of main salt is low prices, is easy to buying, reliable in quality.Plating solution adopts boric acid to be PH buffer reagent, and sodium-chlor is anode activation agent, and these two kinds of solution additives are the additive of nickel plating solution application maturation, reliable and stable.Adopt high-purity sheet nickel of 99.99% as anode, avoid metallic impurity to introduce.
The effect of boric acid is the PH of buffering plating solution, and its content range is relevant with the pH value that plating solution need control, and the concentration range in formula can ensure that the pH value of plating solution is in 5 ~ 6 scopes, and within the scope of this, play good PH shock absorption.The too high levels of boric acid can cause solution pH value to reduce, pH value buffering range offsets to low value, and boric acid content is too low, and cause plating solution pH value to raise, pH value buffering range offsets to high level, plating solution pH value can be caused like this to exceed processing parameter requirement, affect plating solution plating performance.
The effect of sodium-chlor is anode activation agent, prevents anode (sheet nickel) passivation in plating process, promotes that nickel plate normally dissolves.Sodium chloride concentration is too low, well can not ensure the activity of anode nickel plates, passivation phenomenon can occur; Sodium chloride concentration is too high can cause positive plate excessive erosion again, causes the problems such as coating grain raising.
The concentration range of above two kinds of salt is through lot of experiments and contrasts the optimum range applicable of the present invention drawn, can ensure the stability of plating solution, can ensure again the reliability of nickel cobalt coating.
Namely open cylinder plating solution is the plating solution prepared first time, the plating solution of first time plating use.All call off cylinder plating solution according to the new plating solution of recipe requirements preparation at every turn.
One, the control techniques of coating cobalt contents
In electronickelling cobalt liquor system of the present invention, its coating cobalt contents mainly relies on cobalt salt concentration in plating solution to control, and cobalt salt change in concentration, then the cobalt contents deposited in coating also can correspondingly change.In addition, due to two metal ion species that coexist in plating solution (nickel ion and cobalt ion), the sedimentation potential of the two is differentiated, the electropotential of nickel is-0.250V, the electropotential of cobalt is-0.277V, and in plating process, the change of current density also can cause nickel cobalt deposition fraction to change.
The change of above two kinds of factors determines the change of cobalt contents in coating, therefore, studies respectively, draw optimal processing parameter span of control to the cobalt contents corresponding relation in cobalt salt concentration, plating current densities and coating in plating solution.
From accompanying drawing 1, along with the raising of cobalt salt concentration in plating solution, the corresponding raising of the cobalt contents in coating, after in plating solution, cobalt salt concentration reaches 4g/L, the cobalt contents in coating slows down, relatively stable, wherein NiSO
46H
2the content of O is 200g/L, H
3bO
3content be the content of 40g/L, NaCl be 15g/L, plating conditions is: pH is 5, and current density is 1A/dm
2, temperature is 50 DEG C; In conjunction with plating solution cost consideration, opening cobalt salt concentration in cylinder electroplate liquid formulation take 5g/L as the best, both ensured that in coating, cobalt contents was stablized, be convenient to again save cobalt salt consumption, in plating solution, cobalt salt concentration chemical titration analysis method controls, and when plating solution of the present invention and other given parameters of plating conditions are in above-mentioned range, cobalt salt concentration 5g/L is optimum value.
From accompanying drawing 2, in whole current density parameters of test, coating cobalt contents all can meet the requirement of >=10.5%, and therefore, current density parameter is relatively little on the impact of coating cobalt contents comparatively speaking.Current density is at 1.5 ~ 2 A/dm
2in interval, in coating, cobalt contents change steadily, but under exploitation bath system determines, high current density is unfavorable for thickness of coating homogeneity, and lower current densities can cause again Deposit appearance to change, as at 0.5 A/dm
2under current density, there is obfuscation in coating, and has pin hole, wherein NiSO
46H
2the content of O is 200 g/L, H
3bO
3content be the content of 40g/L, NaCl be 15g/L, CoSO
47H
2o 5g/L, plating conditions is: pH is 5, and temperature is 50 DEG C.Synthetic study current density optimum controlling point, with 1 A/dm
2be advisable, under this current density, coating cobalt contents can meet the reliable welding requirements of chip, simultaneously coating depositing homogeneous, well-crystallized, bright appearance.Current density 1 A/dm when plating solution of the present invention and other given parameters of plating conditions are in above-mentioned range
2it is all optimum value.
The present invention's nickel used cobalt coating is the block of the anti-dissimilar metal diffusion applying nickel cobalt coating, is the extraordinary coating developed according to electronic encapsulation shell own material constructional feature and subsequent applications condition.
Electronic encapsulation shell needs to carry out 420 DEG C of sinterable silicon chips, under 420 DEG C of high temperature actions, silicon in silicon can be diffused in the nickel layer of electronic encapsulation shell, cause nickel coating embrittlement cracking, and introduce nickel cobalt coating in electronic encapsulation shell coating after, nickel cobalt coating can prevent the thermodiffusion of silicon, thus prevents from occurring nickel coating brittle cracking problem in shell coating structure, improves its application reliability.
300 DEG C are had in electronic encapsulation shell subsequent applications, the bake process of 30min, with this understanding, nickel in shell nickel layer can be diffused rapidly in the Gold plated Layer of case surface, affects the application of Gold plated Layer function, adds nickel cobalt coating, nickel in nickel cobalt coating can be subject to the constraint of cobalt, can ensure under shell subsequent high temperature application conditions, the diffusion of the layer gold that do not make a difference function, thus improve shell application reliability.
Electronic encapsulation shell is made of a variety of materials, and substantially can be divided into two classes, a class is metallic substance, and common metal is kovar alloy (iron, cobalt, nickelalloy), oxygen free copper; Another kind of is stupalith, and pottery is alumina-ceramic, the tungsten metal paste of surface sintering conduction, and the first plating in tungsten metal paste surface has one deck plating pure nickel or chemical plating nickel-phosphorus alloy, plated nickel cobalt again on it.
The beneficial effect adopting technique scheme to produce is: electroplate liquid of the present invention and plating conditions carry out sample plating, and nickel cobalt coating cobalt contents Absorbable organic halogens is controlled between 15% ~ 30%, can meet the theoretical analysis value requirement of coating cobalt contents >=10.5%.When opening that in cylinder electroplate liquid formulation, cobalt salt concentration is 5g/L, coating cobalt contents is stablized, and is convenient to again save cobalt salt consumption; Current density 1 A/dm
2time coating cobalt contents can meet the reliable welding requirements of chip, coating depositing homogeneous simultaneously, well-crystallized, bright appearance.
Introduce nickel cobalt coating in electronic encapsulation shell coating after, nickel cobalt coating can prevent the thermodiffusion of silicon, thus prevents from occurring nickel coating brittle cracking problem in shell coating structure, improves its application reliability.Nickel in nickel cobalt coating can be subject to the constraint of cobalt, can ensure under shell subsequent high temperature application conditions, the diffusion of the layer gold that do not make a difference function, thus improves shell application reliability.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the corresponding relation curve of plating solution cobalt salt concentration and coating cobalt contents;
Fig. 2 is the homologous thread of current density and coating cobalt contents.
Embodiment
Embodiment 1
A method for electronic encapsulation shell nickel-cobalt alloy plating, comprises the following steps: electronic encapsulation shell to be plated (material is kovar alloy+ceramic tungsten metallization) carries out plating front inspection and preparation before plating by (1); (2) treatment before plating: surface to be plated is cleaned; (3) nickel preplating; (4) nickel plating; (5) nickel plating cobalt: the purity of anode electrolysis nickel plate is 99.99%,
Consisting of of electroplate liquid:
NiSO
4·6H
2O 200 g/l
H
3BO
340g/L
NaCl 15g/L
CoSO
4·7H
2O 5g/L；
Plating conditions is: pH is 5 current densities is 1A/dm
2temperature is 50 DEG C;
(6) gold-plated in advance; (7) gold-plated; (8) aftertreatment.
Nickel cobalt coating cobalt contents is 24.9%, meets the theoretical analysis value requirement of coating cobalt contents >=10.5%.
Embodiment 2
A method for electronic encapsulation shell nickel-cobalt alloy plating, comprises the following steps: electronic encapsulation shell to be plated (material is kovar alloy+ceramic tungsten metallization) carries out plating front inspection and preparation before plating by (1); (2) treatment before plating: surface to be plated is cleaned; (3) nickel preplating; (4) nickel plating; (5) nickel plating cobalt: the purity of anode electrolysis nickel plate is 99.99%,
Consisting of of electroplate liquid:
NiSO
4·6H
2O 180 g/L
H
3BO
345g/L
NaCl 10g/L
CoSO
4·7H
2O 3g/L；
Plating conditions is: pH is 6 current densities is 1.5A/dm
2temperature is 60 DEG C;
(6) gold-plated in advance; (7) gold-plated; (8) aftertreatment.
Nickel cobalt coating cobalt contents is 17.3%, meets the theoretical analysis value requirement of coating cobalt contents >=10.5%.
Embodiment 3
A method for electronic encapsulation shell nickel-cobalt alloy plating, comprises the following steps: electronic encapsulation shell to be plated (material is kovar alloy+ceramic tungsten metallization) carries out plating front inspection and preparation before plating by (1); (2) treatment before plating: surface to be plated is cleaned; (3) nickel preplating; (4) nickel plating; (5) nickel plating cobalt: the purity of anode electrolysis nickel plate is 99.99%,
Consisting of of electroplate liquid:
NiSO
4·6H
2O 220 g/L
H
3BO
335g/L
NaCl 18g/L
CoSO
4·7H
2O 8g/L；
Plating conditions is: pH is 5 current densities is 1A/dm
2temperature is 60 DEG C;
(6) gold-plated in advance; (7) gold-plated; (8) aftertreatment.
Nickel cobalt coating cobalt contents is 26.9%, meets the theoretical analysis value requirement of coating cobalt contents >=10.5%.
Embodiment 4
A method for electronic encapsulation shell nickel-cobalt alloy plating, comprises the following steps: electronic encapsulation shell to be plated (material is kovar alloy+ceramic tungsten metallization) carries out plating front inspection and preparation before plating by (1); (2) treatment before plating: surface to be plated is cleaned; (3) nickel preplating; (4) nickel plating; (5) nickel plating cobalt: the purity of anode electrolysis nickel plate is 99.99%,
Consisting of of electroplate liquid:
NiSO
4·6H
2O 190 g/L
H
3BO
342g/L
NaCl 16g/L
CoSO
4·7H
2O 4g/L；
Plating conditions is: pH is 5.5 current densities is 1.5A/dm
2temperature is 50 DEG C;
(6) gold-plated in advance; (7) gold-plated; (8) aftertreatment.
Nickel cobalt coating cobalt contents is 23.3%, meets the theoretical analysis value requirement of coating cobalt contents >=10.5%.
Embodiment 5
A method for electronic encapsulation shell nickel-cobalt alloy plating, comprises the following steps: electronic encapsulation shell to be plated (material is kovar alloy+ceramic tungsten metallization) carries out plating front inspection and preparation before plating by (1); (2) treatment before plating: surface to be plated is cleaned; (3) nickel preplating; (4) nickel plating; (5) nickel plating cobalt: the purity of anode electrolysis nickel plate is 99.99%,
Consisting of of electroplate liquid:
NiSO
4·6H
2O 210 g/L
H
3BO
338g/L
NaCl 14g/L
CoSO
4·7H
2O 6g/L；
Plating conditions is: pH is 5 current densities is 1A/dm
2temperature is 50 DEG C;
(6) gold-plated in advance; (7) gold-plated; (8) aftertreatment.
Nickel cobalt coating cobalt contents is 24.2%, meets the theoretical analysis value requirement of coating cobalt contents >=10.5%.
Embodiment 6
A method for electronic encapsulation shell nickel-cobalt alloy plating, comprises the following steps: electronic encapsulation shell to be plated (material is kovar alloy+ceramic tungsten metallization) carries out plating front inspection and preparation before plating by (1); (2) treatment before plating: surface to be plated is cleaned; (3) nickel preplating; (4) nickel plating; (5) nickel plating cobalt: the purity of anode electrolysis nickel plate is 99.99%,
Consisting of of electroplate liquid:
NiSO
4·6H
2O 200 g/L
H
3BO
341g/L
NaCl 16g/L
CoSO
4·7H
2O 5g/L；
Plating conditions is: pH is 5 current densities is 1A/dm
2temperature is 50 DEG C;
(6) gold-plated in advance; (7) gold-plated; (8) aftertreatment.
Nickel cobalt coating cobalt contents is 25.3%, meets the theoretical analysis value requirement of coating cobalt contents >=10.5%.
Claims (4)
1. a method for electronic encapsulation shell nickel-cobalt alloy plating, is characterized in that comprising the following steps: (1) carries out plating front inspection and preparation before plating; (2) treatment before plating: surface to be plated is cleaned; (3) nickel preplating; (4) nickel plating; (5) nickel plating cobalt: anode is sheet nickel,
Consisting of of electroplate liquid:
NiSO
4·6H
2O 180～220 g/L
H
3BO
335～45g/L
NaCl 10～18g/L
CoSO
4·7H
2O 3～8g/L；
Plating conditions is: pH is 5 ~ 6 current densities is 1 ~ 2A/dm
2temperature is 50 ~ 60 DEG C;
(6) gold-plated in advance; (7) gold-plated; (8) aftertreatment.
2. the method for electronic encapsulation shell nickel-cobalt alloy plating as claimed in claim 1, is characterized in that: the purity of anode electrolysis nickel plate is 99.99%.
3. the method for electronic encapsulation shell nickel-cobalt alloy plating as claimed in claim 1, is characterized in that: CoSO in electroplate liquid
47H
2the content of O is 5g/L.
4. the method for electronic encapsulation shell nickel-cobalt alloy plating as claimed in claim 1, is characterized in that: current density is 1A/dm
2.
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| CN103510084A (en) * | 2013-09-24 | 2014-01-15 | 宜兴市吉泰电子有限公司 | Preoxidation method of kovar leads for metal housings |
| CN103757674B (en) * | 2013-12-20 | 2017-01-04 | 中国电子科技集团公司第五十五研究所 | A kind of nickel plating process of tungsten-copper composite material |
| CN103911634B (en) * | 2014-03-06 | 2016-09-21 | 中国电子科技集团公司第五十五研究所 | A kind of plating nickel on surface method of molybdenum-base composite material |
| CN109321957B (en) * | 2018-10-24 | 2023-01-17 | 中国电子科技集团公司第五十五研究所 | Environment-friendly shell plating pretreatment etching solution process and plating method |
| CN109628964A (en) * | 2018-12-28 | 2019-04-16 | 浙江长兴电子厂有限公司 | A kind of no lead ceramic package case electroplating technique |
| CN114686942A (en) * | 2022-03-31 | 2022-07-01 | 华源隆精密五金制造(惠州)有限公司 | Production method of high-strength battery shell metal material |
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| CN102618894A (en) * | 2012-04-01 | 2012-08-01 | 昆明理工大学 | Method for preparing thin-wall parts by using electroforming nickel-cobalt alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102618894A (en) * | 2012-04-01 | 2012-08-01 | 昆明理工大学 | Method for preparing thin-wall parts by using electroforming nickel-cobalt alloy |
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| Title |
|---|
| 用于锂离子电池钢壳的镀镍钴钢带制备工艺及耐蚀性研究;李玮;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20120415(第4期);第B022-107页 * |
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