CN106676598B - A method of growth of tin crystal whisker is inhibited based on micro-nano needle wimble structure - Google Patents
A method of growth of tin crystal whisker is inhibited based on micro-nano needle wimble structure Download PDFInfo
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- CN106676598B CN106676598B CN201611149179.2A CN201611149179A CN106676598B CN 106676598 B CN106676598 B CN 106676598B CN 201611149179 A CN201611149179 A CN 201611149179A CN 106676598 B CN106676598 B CN 106676598B
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
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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
- C25D7/00—Electroplating characterised by the article coated
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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
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of methods for inhibiting growth of tin crystal whisker based on micro-nano needle wimble structure, comprising the following steps: one conducting base of selection, and the conducting base is cleaned, after cleaning on the conducting base growth of fine-nano needle wimble structure layer；Then the micro-nano needle wimble structure layer is cleaned, removes surface oxide layer, then grow tin solder on the micro-nano needle wimble structure layer.The present invention has biggish specific surface area and unique geometry using micro-nano needle wimble structure layer, to discharge the compression inside tin coating, to reduce the driving force of tin coating whisker growth, inhibit the formation of tin content, suitable for the growth of various forms of tin layers films, have that preparation method is simple, temperature is low, processing compatibility is strong, the advantages of stability is high, can effectively inhibit the growth of tin layers whisker.
Description
Technical field
The invention belongs to electronic package material technical fields, in particular to a kind of to inhibit tin brilliant based on micro-nano needle wimble structure
The long method of one of the main divisions of the male role in traditional opera.
Background technique
Since tin (Sn) and kamash alloy have good inoxidizability, corrosion resistance and solderability, thus tin coating exists
It is used widely in entire electronics industry, especially electrotinning technology graduallys mature, and tin solder is widely used in
Electronic Packaging field.However, plating tin coating is easy to grow tin content, so as to cause electronic device short circuit and thrashing, sternly
Ghost image rings the reliability of electronic device.
In over the past several decades, causes the report of failure accidents to emerge one after another about tin content, be related to aerospace, nuclear power
Stand, power plant, satellite radar communication etc. key areas.In over the past several decades, the application of Sn-Pb alloy, which becomes, inhibits tin content raw
Long effective ways, but lead is detrimental to health as toxic heavy metal, pollutes environment, is the heavy metal there is an urgent need to substitution
One of.On July 1st, 2006, European Union implement " about the instruction for using certain harmful components in electronic and electrical equipment is limited in "
(Restriction of Hazardous Substances, abbreviation RoHS), and emphasis defines the content of lead no more than
0.1%.Therefore, the defect that pure tin or kamash alloy are easy to grow tin content highlights again, and the micromation pair of electronic device
Tin content proposes more stringent requirement, therefore develops and the new method of growth of tin crystal whisker is inhibited to become urgent problem to be solved.
Currently, the formation mechenism of tin content is not yet clear, but compression as tin content driving force by everybody public affairs
Recognize.Oxidation, interface alloy are total to the generation of compound (IMC), and the structure and pattern and mechanical stress of Sn coating will affect Sn plating
Layer internal stress, to influence the formation of tin content.From the factor for influencing tin content formation, inhibits or weaken tin content and formed
Method mainly have: 1) by alloying, change the ingredient and micro-structure of Sn coating, but in plating alloy technology, ingredient
It controls very difficult.2) formation of oxide is reduced.Such as conformal coating is coated by the surface Sn, it can effectively prevent in a short time
The generation of tin content, but cannot eliminate, and complex process.3) formation of IMC is reduced.Metal substrate especially Cu base is served as a contrast
Bottom prevents the formation of IMC from having positive effect to the inhibition of tin content.4) it flows back or anneals.Reflux or annealing can increase tin crystalline substance
The incubation period of palpus, delay the formation of tin content, but its thermodynamic driving force cannot eliminate, and generate liquid phase and may cause and collapse
It collapses and bridging phenomenon.
As it can be seen that although there are still problems, still not formed generally to fit at present there are the various methods for inhibiting tin content
Mechanism and simple and effective suppressing method.Therefore, it is badly in need of developing a kind of tin simple and effective, suitable for industrial applications
Whisker suppressing method.
Summary of the invention
The present invention in view of the above-mentioned problems existing in the prior art, provides a kind of based on micro-nano needle wimble structure layer inhibition tin
The method of whisker growth discharges the compression inside tin coating using micro-nano needle wimble structure, to reduce tin coating whisker
The driving force of growth inhibits the formation of tin content.Method of the invention overcomes some defects existing for prior art, can keep away
Exempt from reflux or annealing process temperature height thermal damage caused by device, there is low operation temperature, simple process, compatibility are strong, surely
Qualitative height, inhibitory effect clear advantage.
Technical scheme is as follows:
A method of growth of tin crystal whisker is inhibited based on micro-nano needle wimble structure, comprising the following steps:
(1) conducting base is selected, and the conducting base is cleaned, is grown on the conducting base after cleaning
Micro-nano needle wimble structure layer；
(2) then the micro-nano needle wimble structure layer is cleaned, removes surface oxide layer, then in the micro-nano
Tin solder is grown on rice needle wimble structure layer.
Preferably, the conducting base is copper alloy or the pcb board for being deposited with metal layer.
It preferably, include oil removing and pickling to the conducting base cleaning described in step (1)；Step (2) is to described
Micro-nano needle wimble structure layer carry out cleaning include pickling.
Preferably, the height of the micro-nano needle wimble structure layer is 0.2 μm~50 μm.
Preferably, the micro-nano needle wimble structure layer is primary structure or multilevel structure.
Preferably, when the micro-nano needle wimble structure layer is multilevel structure, the size of previous level structure is than rear stage knot
The size of structure is big.
Preferably, the primary structure of the micro-nano needle wimble structure layer is Cu or Ni；The multilevel structure it is last
Primary structure is Ni, Ag or Au.
Preferably, grown on the conducting base micro-nano needle wimble structure layer method be electrodeposition process or
Chemical deposition；Grown on the micro-nano needle wimble structure layer method of the tin solder for plating, chemical plating or
Hot-dip.
Preferably, the tin solder is pure Sn, Sn-Ag, Sn-Ag-Cu or Sn-Zn.
Preferably, the height of the micro-nano needle wimble structure layer not less than the tin solder height four/
One.
Compared with prior art, beneficial effects of the present invention are as follows:
One, a kind of method for inhibiting growth of tin crystal whisker based on micro-nano needle wimble structure of the invention, by elder generation in conductive base
Micro-nano needle wimble structure layer is set on body, since micro-nano needle wimble structure layer has biggish specific surface area and unique geometric form
Shape discharges the compression inside tin coating using micro-nano needle wimble structure layer, to reduce the driving of tin coating whisker growth
Power inhibits the formation of tin content, the growth suitable for various forms of tin layers films；
Two, between conducting base of the invention and micro-nano needle wimble structure layer and micro-nano needle wimble structure layer and tinbase
It is combined by metallic bond between solder, intensity is high, is not easily disconnected from；Method of the invention is simple with preparation method, temperature is low,
The advantages of processing compatibility is strong, and stability is high, can effectively inhibit the growth of tin layers whisker.
Certainly, implement either present invention method not necessarily requiring achieving all the advantages described above at the same time.
Detailed description of the invention
Fig. 1 is the sectional view of the inhibition compound tin layers of growth of tin crystal whisker of the invention.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate this hair
It is bright, rather than limit the scope of protection of the present invention.What those skilled in the art made according to the present invention in practical applications changes
Into and adjustment, still fall within protection scope of the present invention.
As shown in Figure 1, a kind of method for inhibiting growth of tin crystal whisker based on micro-nano needle wimble structure of the invention, including it is following
Step:
(1) conducting base 1 is selected, and to processes such as 1 oil removing of conducting base and pickling, removes conducting base 1
The organic matter and oxide layer on surface, after cleaning on the conducting base 1 growth of fine-nano needle wimble structure layer 2；
(2) processes such as pickling then are carried out to the micro-nano needle wimble structure layer 2, removes surface oxide layer, then in institute
Tin solder 3 is grown on the micro-nano needle wimble structure layer 2 stated.
The conducting base 1 is that copper alloy or the pcb board for being deposited with metal layer etc. have the plating metal on matrix surface
The material of layer.
The method that the micro-nano needle wimble structure layer 2 is grown on the conducting base 1 is electrodeposition process or chemistry
Sedimentation；The method of the tin solder 3 is grown on the micro-nano needle wimble structure layer 2 for plating, chemical plating or heat
Immersion plating.
The height of the micro-nano needle wimble structure layer 2 is 0.2 μm~50 μm, under electro-deposition or chemical deposition, is led to
The parameters such as control additive concentration, sedimentation time, temperature, current density are crossed, to control the height of micro-nano needle wimble structure layer 2；
A quarter of the height of the micro-nano needle wimble structure layer 2 not less than the height of the tin solder 3.
The micro-nano needle wimble structure layer 2 can be primary structure or multilevel structure；When micro-nano needle of the invention is bored
When structure sheaf 2 is primary structure, micro-nano needle wimble structure layer 2 not only can be level-one micron needle wimble structure layer, but also can be level-one
Nanoneedle wimble structure layer, but to guarantee that the height of micro-nano needle wimble structure layer 2 is 0.2 μm~50 μm and not less than the tinbase
The a quarter of the height of solder 3；When the micro-nano needle wimble structure layer 2 is multilevel structure, the size of previous level structure
Size than latter level structure is big, and height is 0.2 μm~50 μm and height is not less than the height of the tin solder 3
A quarter, the multilevel structure can be first grows primary structure 4 in substrate, then raw on the basis of primary structure 4
Long second level or tertiary structure 5.
The primary structure of the micro-nano needle wimble structure layer 2 is the metal member with relatively regular needle taper looks such as Cu or Ni
Element；The afterbody structure of the multilevel structure is that Ni, Ag or Au etc. are not easy to react the member for generating intermetallic compound with Sn
Element.
The tin solder 3 is pure Sn, Sn-Ag, Sn-Ag-Cu or Sn-Zn.
Embodiment 1
It selects lead frame C194 copper alloy for conducting base, to conducting base oil removing 20s, removes 40 DEG C of oil temperature, oil removing
Electric current 3ASD (A/dm2) cleans 20s with 20% dilute sulfuric acid, then deionized water is rinsed well after deionized water is cleaned；It will
The target substrate cleaned up is placed in ready plating solution, and 55 DEG C of solution temperature, the chemical deposition micron copper on conducting base
Needle 20min obtains the copper needle construction that length is 5 μm or so.After deionized water cleaning, it is placed in nickel plating needle plating solution, solution temperature
It is 50 DEG C, current density 1.2ASD, electroplating time 10min, it is 500nm's or so that electro-deposition, which obtains length, on micron copper needle
The micro- cone secondary structure of nickel nanometer.Pickling is carried out to obtained micro-nano needle wimble structure using 20% dilute sulfuric acid, to remove possibility
The aerial oxide layer of exposure, is subsequently placed in tin plating electrolyte, and bath temperature is 25 DEG C, current density 1.0ASD, when plating
Between be 20min, tin thickness be 12 μm or so, be electroplated and cleaning drying carried out to tin layers.
Embodiment 2
It selects stainless steel for conducting base, to conducting base oil removing 30s, removes 40 DEG C of oil temperature, oil removing electric current 4ASD (A/
Dm2), after deionized water is cleaned, 20s is cleaned with 20% dilute sulfuric acid, then deionized water is rinsed well；It is placed in nickel plating needle plating solution
In, solution temperature is 50 DEG C, current density 1.0ASD, electrodeposition time 20min, and it is 700nm or so that electro-deposition, which obtains length,
Nickel nanocone structures.Pickling is carried out to obtained micro-nano needle wimble structure using 20% dilute sulfuric acid, may be exposed with removal
Aerial oxide layer, is subsequently placed in tin plating electrolyte, and bath temperature is 25 DEG C, current density 1.2ASD, and electroplating time is
5min, tin thickness are 2 μm or so, have been electroplated and have carried out cleaning drying to tin layers.
Embodiment 3
It selects semiconductor silicon for matrix, the Cr/Cu seed layer of one layer of 50/500nm is first sputtered on silicon substrate, with 20%
Dilute sulfuric acid cleans 20s, and then deionized water is rinsed well；It is placed in nickel plating needle plating solution, solution temperature is 50 DEG C, current density
1.0ASD, electrodeposition time 20min, electro-deposition obtain the nickel nanocone structures that length is 700nm or so.Using 20% it is dilute
Sulfuric acid carries out pickling to obtained micro-nano needle wimble structure, may expose aerial oxide layer with removal, be subsequently placed in plating
In tin liquor, bath temperature is 25 DEG C, current density 1.2ASD, electroplating time 5min, and tin thickness is 2 μm or so, plating
It is complete that cleaning drying is carried out to tin layers.
In order to evaluate the effect for utilizing micro-nano-tin composite deposite made from the method for the present invention to inhibit growth of tin crystal whisker, this
Invention is tested by the following method: accelerating growth of tin crystal whisker using indentation test, in micro-nano-tin produced by the present invention
The ceramic bead that a diameter is 1mm is placed on composite deposite and pure tin coating (control group) respectively, then on ceramic bead
Apply the constant pressure of 200g, kept for 5 days, humidity is 45~55%, and temperature is 20~25 DEG C, can grow tin crystalline substance in indentation edge
Must, the complexity of coating growth of tin crystal whisker is judged by counting length, diameter and the quantity of indentation edge tin content.Table 1
For the difficulty or ease for evaluating coating growth of tin crystal whisker to Examples 1 to 3 and single tin coating (control group) progress indentation test respectively
Degree.
Table one
As can be seen from Table I, multiple using micro-nano made from the method for the present invention-tin compared to pure tin coating (control group)
It closes coating to have a significant effect to the growth for inhibiting tin content, maximum length, average length, the average diameter sum number of tin content
Amount declines, and the quantity of average length and tin content especially for tin content significantly inhibits, and the present invention passes through
Micro-nano needle wimble structure layer is first introduced on conducting base, and the pressure inside tin coating is discharged using micro-nano needle wimble structure layer and is answered
Power inhibits the formation of tin content to reduce the driving force of tin coating whisker growth.
Conducting base of the invention is not limited to the above pcb board and copper alloy for being deposited with metal layer, on conducting base
The sequence and ingredient for depositing micro-nano needle wimble structure layer can exchange, but guarantee the needle cone cell pattern of micro nano structure layer, most
The micro nano structure ingredient of rear stage should be not likely to produce intermetallic compound with tin layers, and the growing method of tin layers is not limited to electricity
Plating, or chemical plating, hot-dip.The temperature of electro-deposition or chemical deposition, current density, sedimentation time can be according to reality
Operation voluntarily adjusts.Those skilled in that art's made any variation and adjustment within foregoing invention design, belongs to this
In the protection scope of application.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (8)
1. a kind of method for inhibiting growth of tin crystal whisker based on micro-nano needle wimble structure, which comprises the following steps:
(1) select a conducting base, and the conducting base cleaned, after cleaning on the conducting base growth of micro-nano
Rice needle wimble structure layer；
(2) then the micro-nano needle wimble structure layer is cleaned, removes surface oxide layer, then in the micro-nano needle
Tin solder is grown on wimble structure layer；
The micro-nano needle wimble structure layer is primary structure or multilevel structure；The level-one knot of the micro-nano needle wimble structure layer
Structure is Cu or Ni；
The afterbody structure of the multilevel structure is Ni, Ag or Au.
2. a kind of method for being inhibited growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, feature are existed
In the conducting base is copper alloy or the pcb board for being deposited with metal layer.
3. a kind of method for being inhibited growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, feature are existed
In cleaning described in step (1) to the conducting base includes oil removing and pickling；Step (2) bores the micro-nano needle
It includes pickling that structure sheaf, which carries out cleaning,.
4. a kind of method for being inhibited growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, feature are existed
In the height of the micro-nano needle wimble structure layer is 0.2 μm~50 μm.
5. a kind of method for being inhibited growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, feature are existed
In when the micro-nano needle wimble structure layer is multilevel structure, the size of previous level structure is bigger than the size of latter level structure.
6. a kind of method for being inhibited growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, feature are existed
In the method for growing the micro-nano needle wimble structure layer on the conducting base is electrodeposition process or chemical deposition；
The method of the tin solder is grown on the micro-nano needle wimble structure layer for plating, chemical plating or hot-dip.
7. a kind of method for being inhibited growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, feature are existed
In the tin solder is pure Sn, Sn-Ag, Sn-Ag-Cu or Sn-Zn.
8. a kind of method for being inhibited growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, feature are existed
In the height of the micro-nano needle wimble structure layer is not less than a quarter of the height of the tin solder.
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| CN108914170B (en) * | 2018-06-21 | 2021-04-02 | 上海芮远化学科技有限公司 | Composite electroplating solution, preparation method of composite electroplating solution and electroplating method |
| CN109722683B (en) * | 2019-01-04 | 2020-09-25 | 中国科学院合肥物质科学研究院 | Gold nanostructure with conical surface and preparation method and application thereof |
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| CN106414808A (en) * | 2014-06-11 | 2017-02-15 | 上村工业株式会社 | Tin electroplating bath and tin plating film |
| CN104112681A (en) * | 2014-07-03 | 2014-10-22 | 上海交通大学 | Solid-state ultrasonic bonding method based on copper microneedle cone |
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