CN105984177A - Composite coated film, preparing method thereof and electronic element - Google Patents
Composite coated film, preparing method thereof and electronic element Download PDFInfo
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- CN105984177A CN105984177A CN201510086618.9A CN201510086618A CN105984177A CN 105984177 A CN105984177 A CN 105984177A CN 201510086618 A CN201510086618 A CN 201510086618A CN 105984177 A CN105984177 A CN 105984177A
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Abstract
The invention provides a composite coated film. The composite coated film is located on a base material and comprises multiple semigloss tin coated films and a nickel blocking layer located between the multiple semigloss tin coated films and the base material, in the direction from the base material to the top surface of the multiple semigloss tin coated films, the multiple semigloss tin coated films comprise a first tin coated layer and a second tin coated layer which are sequentially alternately overlapped from the bottom layer to the top layer, the first tin coated layer is formed by electroplating with first-current-density, and the second tin coated layer is formed by electroplating with second-current-density. Under the thermocycling and/or high-temperature damp and hot conditions, the composite coated film can still effectively inhibit growth of crystal whiskers on the tin coated layers.
Description
Technical field
The present invention relates to stannum electroplating film field, in particular to stannum electroplating film and the preparation thereof of anti-whisker growth
Method.
Background technology
Pure tin coating well can merge with unleaded eutectic alloy Sn-Ag-Cu solder due to it, and still can continue to use
The production equipment of tin-lead coating and production line in the past, the advantages such as Financial cost is relatively low and get the attention,
It is widely used in IC pin, adapter or bus.But pure tin coating replaces tin-lead coating to need to solve
Critical problem be exactly stannum must autonomous growth.Stannum must be spontaneous at pure tin or kamash alloy coating surface
The monocrystal of a kind of elongated stannum grown, the existence of stannum palpus can cause adjacent welds or lead short circuit to draw
Send out fault so that performance and the life-span of electric element are remarkably decreased, and make miniaturization of electronic products trend
Become serious to hinder.
Stannum one of the main divisions of the male role in traditional opera's length can be by just can effectively suppress brilliant after the Pb alloying of interpolation about 3% in Sn in the past
One of the main divisions of the male role in traditional opera's length, has inhibition, and its coating stress level ratio mainly due to Pb to the crystal boundary migration of Sn
Pure tin is much lower, and the IMC speed of growth of interface is also slow compared with pure tin.But due to Europe WEEE and
RoHS prohibits the use of toxic element Pb's etc., and electronic packaging industry initially enters the unleaded epoch, therefore must
Other alternative methods must be researched and developed.
[B.Horvath, B.Illes, T.Shinohara, G.Harsanyi, the Thin Solid Films 520 such as Horvath
(2011)384；M.N.Chen,S.J.Ding,Q.Q.Sun,D.W.Zhang,L.K.Wang,J.Electron.
Mater.37(2008)894.；A.Dimitrovska,R.Kovacevic,J.Electron.Mater.38(2009)
2516；Y.Wang,D.Ding,T.Liu,K.P.Galuschki,Y.Hu,A.Gong,S.Bai,M.Li,D.
Mao, ICEPT-HDP (2010) 980] think one layer of nickel barrier layer of preplating on parent metal such as copper alloy, then
Plating solderability pure tin coating can substantially suppress the growth of whisker, and the existence mainly due to barrier layer prevents
Matrix element Cu spreads in Sn coating, reduces the response speed at Cu/Sn interface, simultaneously nickel barrier layer
Mainly present stannum one of the main divisions of the male role in traditional opera's length i.e. tension of disadvantageous reversal of stress, reach to reduce stannum palpus growth driving force
Purpose.Suggestion pre-nickel plating thickness should be not less than 0.5 μm in the world.Further, the preplating disclosed in prior art
Nickel dam is generally used for reducing the crack caused when molded lead frame bends and generates, and in hygrothermal environment condition
Under, particularly under the conditions of cold cycling, stannum one of the main divisions of the male role in traditional opera length is more serious.It is thus desirable to one can be to heat resistance ring
The method of the stannum one of the main divisions of the male role in traditional opera's length under the conditions of border and cold cycling.
Summary of the invention
In order to suppress tin coating whisker growth under cold cycling and/or high temperature wet heat condition, the present invention provides
A kind of composite film coating, it comprises multilayer matte tin plated film and is positioned at the nickel under described multilayer matte tin plated film
Barrier layer, wherein said multilayer matte tin plated film includes plating with this first stannum replacing superposition from bottom to top layer
Layer and the second tin coating, described first tin coating is formed with the first electric current density plating, described second tin coating
Formed with the second electric current density plating less than the first electric current density.Hot and humid condition generally refers to
Under the relative humidities of 85%RH or above, temperature is more than 55 DEG C, such as in the range of 55 DEG C to 85 DEG C
Condition, can be the use condition of storage condition, more preferably electronic component.By nickel barrier layer with many
Layer being applied in combination of matte tin plated film, enhance cold cycling and hot and humid under the conditions of anti-whisker growth
Ability so that it is be resistant to the hot and humid storage condition of longer time, and coated surface is more smooth,
Avoid the appearance of pit and crackle.Described multilayer matte tin plated film can be two-layer or three layers, by utilizing
Different electric current density plating makes stannum plated film be layered, and can regulate the grain size of plated stannum, thus discharge
Stress, it is to avoid the generation of stannum palpus.
In one preferred embodiment, in described multilayer matte tin plated film, the stannum purity of each layer is at least
99.9wt%, preferably at least 99.95wt%, remaining is impurity, and impurity mainly includes carbon, oxygen, copper, ferrum, phosphorus
Deng, it is essentially from additive such as methanesulfonic acid, the leveling agent etc. in base material and following plating solution.Highly purified stannum
Ensure that its solderability, and owing to being substantially free of lead, decrease the pollution to environment.The stannum that purity is the highest
Although whisker growth is less, but the conditions such as the solderability required as tin coating itself can not be met.
In one preferred embodiment, described nickel barrier layer thickness is less than 0.5 micron.Inventor is unexpected
Finding, when nickel barrier layer thickness is less than 0.5 micron, the effect of its suppression whisker becomes apparent from, and less
Pit and crackle occur, so that coated surface is more smooth.Additionally, the nickel coating more than 0.5 micron exists
It is more prone to cracking on the pin of bending, thus affects tin coating further, the cracking of tin coating may be caused.
In a preferred embodiment, the thickness summation of described multilayer matte tin plated film is 6 microns.In order to
The most anti-stannum one of the main divisions of the male role in traditional opera's length, traditional solderability tin coating thickness that industry uses is generally 8～10 microns,
The present invention by utilizing the combination of nickel barrier layer and multilayer matte tin plated film to reduce further tin coating thickness,
Thus provide cost savings further.
In one preferred embodiment, described first electric current density is at 5 to 25A/dm2In the range of, excellent
Elect 10 to 20A/dm as2, more preferably 13 to 18A/dm2；And described second electric current density be 2.5 to
20A/dm2In the range of, preferably 5 to 15A/dm2, more preferably 8 to 12A/dm2.First electric current density
It is preferably 2 to 10A/dm with the difference of the second electric current density2, more preferably 4 to 8A/dm2, particularly preferably
About 5A/dm2.The first electric current density used when electroplating each layer the first tin coating can be identical or different, only
The second electric current density wanting the second tin coating to be used is less than first that the first tin coating adjacent thereto is used
Electric current density.If known in the art tin plating time electric current density low, then crystallize exquisiteness, softness, deposition velocity
Slowly, but production efficiency is low；It is high that electric current density height then crystallizes thick (burn time serious, powder), hardness,
But deposition velocity is fast, production efficiency is high.Inventor combines the above-mentioned electric current density of each side selecting factors, obtains
There is the tin coating of more preferable crystallographic property and configuration of surface, and can have higher production efficiency.
Present invention also offers the method preparing above-mentioned composite film coating, described method comprises the steps: at base
Nickel barrier layer is formed on material；Nickel barrier layer forms the first tin coating with the first electric current density plating；?
The second tin coating is formed with the second electric current density less than the first electric current density on one tin coating；Alternatively,
Second tin coating is repeated in as required form the first tin coating and the second tin coating.
In one preferred embodiment, described first electric current density is at 5 to 25A/dm2In the range of, excellent
Elect 10 to 20A/dm as2, more preferably 13 to 18A/dm2；And described second electric current density be 2.5 to
20A/dm2In the range of, preferably 5 to 15A/dm2, more preferably 8 to 12A/dm2.First electric current density
It is preferably 2 to 10A/dm with the difference of the second electric current density2, more preferably 4 to 8A/dm2, particularly preferably
About 5A/dm2.The first electric current density used when electroplating each layer the first tin coating can be identical or different, only
The second electric current density wanting the second tin coating to be used is less than first that the first tin coating adjacent thereto is used
Electric current density.If known in the art tin plating time electric current density low, then crystallize exquisiteness, softness, deposition velocity
Slowly, but production efficiency is low；Electric current density height then crystallizes thick (burning time serious or in powder), hardness
Height, but deposition velocity is fast, and production efficiency is high.Inventor combines the above-mentioned electric current density of each side selecting factors,
Obtain the tin coating with more preferable crystallographic property and configuration of surface, and can have higher production efficiency.
Invention further provides a kind of electronic component, above-mentioned compound including on base material and described base material
Plated film.
In one preferred embodiment, described base material by plastics, resin, copper and copper alloy extremely
Few a kind of material is made.
In one preferred embodiment, described electronic component is selected from lead frame, ic package, core
Piece element, adapter and bus.
Accompanying drawing explanation
Fig. 1 is the atomic force microscope photo on different-thickness nickel barrier layer, the wherein thickness on nickel barrier layer
It is respectively (a) 1 μm, (b) 0.5 μm, (c) 0.1 μm, (d) 0.05 μm.Substrate metal is the C194 of rolling
Alloy foil sheet, microcosmic surface has scraggly rolling vestige, along with the increase of electronickelling barrier layer thickness,
Rolling vestige fades away and tends to smooth；
Fig. 2 is the scanning electron microscope sem photo of the surface topography of double-deck matte tin (3 μm/3 μm) coating, nickel
Barrier layer thickness is respectively (a) 0.5 μm, (b) 0.1 μm, (c) 0.05 μm；
Fig. 3 is the surface topography of the comparative example 1 and 2 after 2000 cold cycling tests, and it all have employed
10 μ m-thick Asia light Sn coating, its respective nickel barrier layer thickness is respectively (a): 1 μm (comparative example 1),
(b): 0.05 μm (comparative example 2)；
Fig. 4 is the composite deposite surface of the exemplary embodiment of the invention after 2000 cold cycling tests
Pattern, all uses 6 μ m-thick monolayer Asia light Sn coating (1 μm/5 μm), and its nickel barrier layer thickness is respectively
(a) 1 μm (embodiment 1), (b) 0.05 μm (embodiment 2)；
Fig. 5 is the composite deposite table of the exemplary embodiment of the invention after 2000 cold cycling tests
Face pattern, all uses sub-light bilayer Sn coating (1 μm/5 μm), and nickel barrier layer thickness is respectively (a) 1 μm
(embodiment 1), (b) 0.05 μm (embodiment 2)；
Fig. 6 is the composite deposite table of the exemplary embodiment of the invention after 2000 cold cycling tests
Face pattern, all uses sub-light bilayer Sn coating (3 μm/3 μm), and nickel barrier layer thickness is respectively (a) 0.5 μm
(embodiment 3), (b) 0.1 μm (embodiment 4), (c) 0.05 μm (embodiment 5)；
Fig. 7 is answering of the exemplary embodiment of the invention after 85 DEG C/85%RH storage in 2000 hours
Closing coating surface morphology, all use double-deck Sn (3 μm/3 μm) coating, nickel barrier layer thickness is respectively (a)
0.5 μm (embodiment 3), (b) 0.1 μm (embodiment 4), (c) 0.05 μm (embodiment 5)；
Fig. 8 is the matte tin plated film of PCB sample table after-40 DEG C to 125 DEG C of thermal cycles test 3000 times
Face pattern, as a comparison case 5.
Detailed description of the invention
Below in association with specific embodiment, embodiments of the present invention are carried out exemplary description, but these are real
Execute example and be not meant to any degree limiting the scope of the present invention.
In this article, the term that illustrates to be used during position relationship " on " D score etc., its phase para-position referred to
Put relation rather than absolute " on " or the position of D score, it will be understood by those skilled in the art that its indication
The technical scheme in generation.
Present invention applicant in patent CN103317790A it is proposed that be prepared for multilayer matte pure tin coating,
Find that the double-deck matte tin film that electric current density is different has certain inhibitory action to stannum one of the main divisions of the male role in traditional opera's length.In order to further
Strengthen cold cycling and hot and humid under the conditions of the ability of anti-whisker growth, this invention takes with above-mentioned pair
Layer stannum film is as can layer and based on nickel aminosulfonic bath preparing between layer and copper substrate material
Nickel barrier layer adds the double inhibition measure of high inhibition stannum one of the main divisions of the male role in traditional opera's length.In the prior art, nickel barrier layer is general
The crack being used for causing when reducing molded lead frame bending under normal temperature condition generates, and is often therefore commonly used in
In the electronic component that temperature uses.And for needing the electronic component used in the environment of the most harsh, such as
Under conditions of hot and humid condition or cold cycling, its stannum one of the main divisions of the male role in traditional opera's length or problem are more serious, it is therefore desirable to
The electronic component avoiding stannum one of the main divisions of the male role in traditional opera's length of hot and humid condition or cold cycling can be resisted.In research process,
Inventor is found that while that preplating 1 μm nickel coating can reach suppression whisker growth under the conditions of hygrothermal environment, but
It is that its stannum one of the main divisions of the male role in traditional opera length under the conditions of cold cycling is more serious.And inventors be surprised to learn that, when nickel barrier layer and basis
When the multilayer matte tin plated film of invention is applied in combination, not only decreases the formation in crack, also enhance it cold
Thermal cycle conditions and hot and humid under the conditions of the ability of anti-stannum one of the main divisions of the male role in traditional opera's length.
Particularly in the case of nickel barrier layer is less than or equal to 0.5 micron, it is possible to obtain more smooth stannum plated film
Surface, even and if experience cold cycling many times, such as more than 2,000 times, remain able to suppress whisker
Growth.And decrease whisker and come off the appearance of the pit caused and the generation of crackle.
Preparation example
According to one embodiment of the present invention, prepare a kind of high inhibition pure tin coating surface stannum one of the main divisions of the male role in traditional opera's length that adds
Double-deck stannum and the composite deposite on nickel barrier layer, while environment resistant stannum one of the main divisions of the male role in traditional opera's length, decrease the thickness of pure tin coating
Degree.
The electroplating deposition on nickel barrier layer:
The preparation on nickel barrier layer provided by the present invention is electroplated according to electroplate liquid formulation and the parameter of table 1.
Table 1 nickel aminosulfonic bath formula and experiment condition
Then on nickel barrier layer, the double-deck matte tin plated film of deposition.This preparation example employs number of patent application
The plating solution of CN103317790A and the double-deck tin coating of technique preparation, ground floor (bottom) electric current density is
15A/dm2, the second layer (top layer) stannum electric current density is 5A/dm2, it is 1 μm (top layer)/5 μm that thickness separately designs
(bottom), 3 μm (top layer)/3 μm (bottom), gross thickness is 6 μm.Use Shanghai newly sun quasiconductor
The high speed matte tin plating solution of Materials Co., Ltd (comprise 170mL/L SYT820,50mL/LSYT5370,
180mL/L SYT810), electroplating temperature is 40 DEG C.For the most anti-stannum one of the main divisions of the male role in traditional opera's length, industry is adopted
Traditional solderability tin coating thickness be generally 8～10 μm, say from solderability angle, not less than 6 μm
Reaching solderability requirement, the double-deck stannum of 6 μ m-thick again can be the most cost-effective.
The surface topography on AFM test different-thickness Ni barrier layer.Fig. 1 is the AFM on different-thickness nickel barrier layer
Photo.Substrate metal is the C194 alloy foil sheet of rolling, and microcosmic surface has scraggly rolling vestige,
Along with the increase of electronickelling barrier layer thickness, rolling vestige fades away and tends to smooth.
Fig. 2 is electroplating double-layer Sn coating surface morphology photo on different-thickness nickel barrier layer, and surface is all compared
Smooth do not affected by nickel barrier layer pattern.Ni and the Sn thickness of coating of the plating of each embodiment and comparative example
Record is measured in table 2 by X-ray thickness gauge.
Evaluation Example
Method of testing:
Use damp and hot test (TH) and cold cycling (TCT) test crystalline substance to multilamellar stannum film in the present invention
Inhibition must be simulated test.Before test, respectively nickel dam and double-deck matte tin plated film are deposited on
On the plane C194 lead frame alloy of punching, anneal 1 hour at 150 DEG C, the most respectively to annealing
Aspect product carry out damp and hot test and cold cycling test.
The damp and hot test of the double-deck stannum sample of nickel preplating: 85 DEG C and 85%RH hot and humid under the conditions of deposit
Store up 2000 hours.55 DEG C/85%RH hot and humid under the conditions of store 4000 hours.
The cold cycling test of the double-deck stannum sample of nickel preplating: complete to circulate 2000 at-55 DEG C to 125 DEG C
Secondary, all continue 10 minutes when high temperature and low temperature.
Field emission electron scanning microscope (FEI Siron200) is used to observe sample under 50-50000 amplification
Product surface topography.
Test result is shown in Table 2.
Table 2 sample parameters and TCT and TH test result.
Seeing table 2 and Fig. 3 to Fig. 8 visible, (double-deck matte tin coating hinders the composite film coating of the present invention with nickel
The combination of barrier) it is resistant to the hot and humid environment of longer time and more cold cycling, without
Produce whisker, crackle etc. and affect the defect of coating character.Double-deck matte tin (1 μm, 5ASD/5 μm, 15ASD)
The composite deposite combined with nickel barrier layer (1 μm) all can substantially press down under cold cycling and high temperature wet heat condition
Tin coating surface processed whisker growth.Double-deck sub-light Sn (3 μm, 5ASD/3 μm, 15ASD) and ultra-thin Ni resistance
The sample that barrier (0.05～0.1 μm) combines, can reduce the risk of growth of tin crystal whisker after thermal cycling significantly,
Coating surface is made seldom to occur in the patterns such as the surface crater brought in Thermal Cycling and crackle due to thermal stress
Change.
Specifically, after 2000 cold cycling tests, when all there is the nickel barrier layer of 1 micron, right
For 10 traditional μ m-thick monolayer Asia light Sn coating, compared with double-deck matte tin coating, hence it is evident that have
More stannum must (comparative example 1, in Fig. 3 a), and there is the double-deck sub-light on the nickel barrier layer of same thickness
(embodiment 1, the stannum that a) then do not has in Fig. 5 must occur tin coating；When nickel barrier layer is relatively thin, can subtract
Few TCT cold cycling process produces density and the length (seeing Fig. 3) of whisker.Traditional sub-light Sn coating
Thickness reduces to 6 μm, and after the test of TCT cold cycling, whisker density substantially reduces (Fig. 4).Relatively thin Ni (0.05
μm) sample surfaces more they tend to smooth, pit and crackle (Fig. 3 b, Fig. 4 b and Fig. 5 b) less occur, especially
It is the sample of double-deck matte tin plated film and ultra-thin nickel barrier combination.Use simultaneously double-deck matte tin plated film and
The sample on ultra-thin nickel barrier layer, after experienced by 2000 cold cycling, does not has whisker to occur the most substantially,
And surfacing (Fig. 5 and Fig. 6).
After experience 85 DEG C/85%RH storage in 2000 hours, the composite film coating of the present invention still presents excellence
Surface topography, does not has the appearance of whisker, pit and crackle, it is possible to meet the needs of the actual application of electronic component.
It addition, as a comparison case 5, test the double-deck matte tin plated film (without nickel barrier layer) of PCB sample
Surface topography after-40 DEG C to 125 DEG C of thermal cycles test 3000 times, finds the sample not having nickel barrier layer,
The appearance of whisker can also not be had, to 2000 circulations and 3000 circulations when 1300 cold cycling
Time, it can be seen that there is (in Fig. 8 part) indicated by circle in significantly crackle, and has fraction of whisker
(seeing Fig. 8).
As fully visible, multilayer matte tin plated film can be resisted sternly to greatest extent with the combination on ultra-thin nickel barrier layer
Severe environment without producing whisker, pit and crackle, thus meets the various need of electronic component to its impact
Want.
Claims (9)
1. composite film coating, described composite film coating is positioned on base material, and comprises multilayer matte tin plated film and be positioned at institute
State the nickel barrier layer between multilayer matte tin plated film and described base material, wherein from base material to described multilayer matte
On the direction of tin-plated coating film top surface, described multilayer matte tin plated film includes replacing successively superposition from bottom to top layer
The first tin coating and the second tin coating, described first tin coating with first electric current density plating formed, described
Second tin coating is formed with the second electric current density plating less than the first electric current density.
2. composite film coating as claimed in claim 1, in wherein said multilayer matte tin plated film, the stannum of each layer is pure
Degree is at least 99.9wt%.
3. composite film coating as claimed in claim 1 or 2, the thickness of wherein said multilayer matte tin plated film is total
With for 6 microns.
4. composite film coating as claimed in claim 1, wherein said first electric current density is at 5 to 25A/dm2
In the range of, and described second electric current density is 2.5 to 20A/dm2In the range of.
5. composite film coating as claimed in claim 1, wherein said nickel barrier layer thickness is less than 0.5 micron.
6. the method for preparation composite film coating as according to any one of claim 1 to 5, described method includes
Following steps:
Base material is formed nickel barrier layer；
Nickel barrier layer forms the first tin coating with the first electric current density plating；
First tin coating forms the second tin coating with the second electric current density less than the first electric current density；With
Alternatively, the second tin coating is repeated in as required form the first tin coating and the second tin coating.
7. an electronic component, including on base material and described base material as any one of claim 1 to 5
Described composite film coating.
8. electronic component as claimed in claim 7, wherein said base material by selected from plastics, resin, copper and
In copper alloy, the material of at least one is made.
9. electronic component as claimed in claim 7, wherein said electronic component is lead frame, semiconductor package
Dress thing, chip component, adapter or bus.
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| CN201510086618.9A CN105984177B (en) | 2015-02-17 | 2015-02-17 | Composite film coating, preparation method and electronic component |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112342575A (en) * | 2020-09-10 | 2021-02-09 | 安徽龙芯微科技有限公司 | Electroplating method of semiconductor packaging piece |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940137A (en) * | 2001-01-31 | 2007-04-04 | 同和矿业株式会社 | Heat resistant film, its manufacturing method, and electrical and electronic parts |
| CN101108546A (en) * | 2007-08-30 | 2008-01-23 | 山东天诺光电材料有限公司 | Flexible material and method of manufacturing the same and use thereof |
| CN101908515A (en) * | 2009-06-08 | 2010-12-08 | 瑞萨电子株式会社 | Semiconductor device and preparation method thereof |
| CN103317790A (en) * | 2012-03-19 | 2013-09-25 | 西门子公司 | Multilayer matte tin plated film and preparation method thereof |
| WO2014048414A1 (en) * | 2012-09-26 | 2014-04-03 | Harting Kgaa | Electrical contact element |
-
2015
- 2015-02-17 CN CN201510086618.9A patent/CN105984177B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940137A (en) * | 2001-01-31 | 2007-04-04 | 同和矿业株式会社 | Heat resistant film, its manufacturing method, and electrical and electronic parts |
| CN101108546A (en) * | 2007-08-30 | 2008-01-23 | 山东天诺光电材料有限公司 | Flexible material and method of manufacturing the same and use thereof |
| CN101908515A (en) * | 2009-06-08 | 2010-12-08 | 瑞萨电子株式会社 | Semiconductor device and preparation method thereof |
| CN103317790A (en) * | 2012-03-19 | 2013-09-25 | 西门子公司 | Multilayer matte tin plated film and preparation method thereof |
| WO2014048414A1 (en) * | 2012-09-26 | 2014-04-03 | Harting Kgaa | Electrical contact element |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112342575A (en) * | 2020-09-10 | 2021-02-09 | 安徽龙芯微科技有限公司 | Electroplating method of semiconductor packaging piece |
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