CN106676598A - A method for restraining tin whisker growing based on micro-nano cone structure - Google Patents
A method for restraining tin whisker growing based on micro-nano cone structure Download PDFInfo
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- CN106676598A CN106676598A CN201611149179.2A CN201611149179A CN106676598A CN 106676598 A CN106676598 A CN 106676598A CN 201611149179 A CN201611149179 A CN 201611149179A CN 106676598 A CN106676598 A CN 106676598A
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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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a method for restraining tin whisker growing based on a micro-nano cone structure. The method comprises the following steps that a conductive matrix is selected and cleaned; after the matrix is cleaned, a micro-nano cone structure layer grows on the conductive matrix; then the micro-nano cone structure layer is cleaned, and a surface oxide layer is removed; and finally, tin-based welding flux grows on the micro-nano cone structure layer. According to the method, the pressure stress in a tin cladding layer is released by utilizing the fact that the micro-nano cone structure layer has a large specific surface area and a unique geometrical shape, driving force for tin cladding layer tin cladding layer is reduced, and formation of tin whisker is restrained; the method is suitable for growing of various types of tin layer thin films and has the advantages that the preparation method is simple, the temperature is low, compatibility of the technique is high, stability is high, and growing of tin whiskers can be effectively restrained.
Description
Technical field
The invention belongs to electronic package material technical field, more particularly to a kind of to suppress stannum brilliant based on micro-nano needle wimble structure
The method of one of the main divisions of the male role in traditional opera's length.
Background technology
Because stannum (Sn) and kamash alloy have good non-oxidizability, corrosion resistance and solderability, thus tin coating exists
It is used widely in whole electron trade, particularly electrotinning Technology is gradually ripe, 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, cause the report of failure accidents to emerge in an endless stream with regard to tin content, be related to Aero-Space, nuclear power
Stand, power plant, satellite radar communication etc. key areas.In over the past several decades, the application of Sn-Pb alloys becomes suppression tin content life
Long effective ways, but lead is used as toxic heavy metal, is detrimental to health, and pollutes environment, is the heavy metal in the urgent need to substituting
One of.On July 1st, 2006, European Union implements《The instruction of some harmful components used in regard to being limited in electronic and electrical equipment》
(Restriction of Hazardous Substances, abbreviation RoHS), and emphasis defines the content of lead no more than
0.1%.Therefore, pure tin or kamash alloy are easy to grow the defect of tin content and highlight again, and the miniaturization of electronic device is right
Tin content proposes more stringent requirement, therefore exploitation suppresses the new method of growth of tin crystal whisker to become problem demanding prompt solution.
At present, the formation mechenism of tin content is not yet clear, but compressive stress as tin content driving force by everybody public affairs
Recognize.Oxidation, the generation of the common compound (IMC) of interface alloy, the structure and pattern of Sn coating, and mechanical stress can affect Sn to plate
Layer internal stress, so as to affect the formation of tin content.From the factor for affecting tin content to be formed, suppress or weaken tin content and formed
Method mainly have：1) by alloying, the composition and micro structure of Sn coating is changed, but in plating alloy technology, composition
Control is very difficult.2) formation of oxide is reduced.For example by Sn surface-coated conformal coatings, can effectively prevent in a short time
The generation of tin content, but can not eliminate, and complex process.3) formation of IMC is reduced.For metal substrate is particularly Cu bases lining
Bottom, prevents suppression of the formation of IMC to tin content from having positive effect.4) flow back or anneal.It is brilliant that backflow or annealing can increase stannum
Must stage of incubation, delay the formation of tin content, but its thermodynamic driving force can not be eliminated, and produced liquid phase and may be caused to collapse
Collapse and bridging phenomenon.
It can be seen that, although the method that there are various suppression tin contents at present, still suffers from problems, do not formed generally fit yet
Mechanism, and simple and effective suppressing method.Therefore, it is badly in need of a kind of simple stannum that is effective, being suitable to industrial applications of exploitation
Whisker suppressing method.
The content of the invention
The problems referred to above that the present invention exists for prior art, there is provided one kind suppresses stannum based on micro-nano needle wimble structure layer
The method of whisker growth, the compressive stress inside tin coating is discharged using micro-nano needle wimble structure, so as to reduce tin coating whisker
The driving force of growth, suppresses the formation of tin content.The method of the present invention overcomes some defects of existing process presence, can keep away
Exempt from the hot injury for flowing back or annealing process temperature height is caused to device, low with operation temperature, process is simple, compatibility are strong, surely
Qualitative height, inhibition clear advantage.
Technical scheme is as follows：
A kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure, comprises the following steps：
(1) conducting base is selected, and described conducting base is cleaned, grown on described conducting base after cleaning
Micro-nano needle wimble structure layer；
(2) and then to described micro-nano needle wimble structure layer clean, remove surface oxide layer, then in described micro-nano
Tin solder is grown on rice pin wimble structure layer.
Preferably, described conducting base is the pcb board that copper alloy or deposition have metal level.
Preferably, oil removing and pickling are included to described 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 described micro-nano needle wimble structure layer is 0.2 μm~50 μm.
Preferably, described micro-nano needle wimble structure layer is primary structure or multilevel hierarchy.
Preferably, when described micro-nano needle wimble structure layer is multilevel hierarchy, the size of previous level structure is tied than rear stage
The size of structure is big.
Preferably, the primary structure of described micro-nano needle wimble structure layer is Cu or Ni；Described multilevel hierarchy it is last
Primary structure is Ni, Ag or Au.
Preferably, the method that described micro-nano needle wimble structure layer is grown on described conducting base be electrodeposition process or
Chemical deposition；The method that described tin solder is grown on described micro-nano needle wimble structure layer is plating, chemical plating or
Hot-dip.
Preferably, described tin solder is pure Sn, Sn-Ag, Sn-Ag-Cu or Sn-Zn.
Preferably, the height of described micro-nano needle wimble structure layer be not less than the height of described tin solder four/
One.
Compared with prior art, beneficial effects of the present invention are as follows：
First, a kind of method that growth of tin crystal whisker is suppressed 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, because micro-nano needle wimble structure layer has the geometric form of larger specific surface area and uniqueness
Shape, the compressive stress inside tin coating is discharged using micro-nano needle wimble structure layer, so as to reduce the driving of tin coating whisker growth
Power, suppresses the formation of tin content, it is adaptable to the growth of various forms of tin layers thin film；
2nd, between conducting base of the invention and micro-nano needle wimble structure layer, and micro-nano needle wimble structure layer and tinbase
Combined by metallic bond between solder, intensity is high, is not easily disconnected from；The method of the present invention has that preparation method is simple, temperature is low,
Processing compatibility is strong, and stability is high, can effectively suppress the advantage of the growth of tin layers whisker.
Certainly, the either method for implementing the present invention it is not absolutely required to while reaching all the above advantage.
Description of the drawings
Fig. 1 is that the growth of tin crystal whisker that suppresses of the present invention is combined the profile of tin layers.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate this
It is bright, rather than limit protection scope of the present invention.In actual applications those skilled in the art are according to changing that the present invention makes
Enter and adjust, still fall within protection scope of the present invention.
As shown in figure 1, a kind of method that growth of tin crystal whisker is suppressed based on micro-nano needle wimble structure of the present invention, including it is following
Step：
(1) conducting base 1 is selected, and to processes such as the described oil removings of conducting base 1 and pickling, removes conducting base 1
The Organic substance and oxide layer on surface, after cleaning on described conducting base 1 growth of fine-nano pin wimble structure layer 2；
(2) processes such as pickling and then to described micro-nano needle wimble structure layer 2 are carried out, surface oxide layer is removed, then in institute
Tin solder 3 is grown on the micro-nano needle wimble structure layer 2 stated.
Described conducting base 1 be copper alloy or deposition have pcb board of metal level etc. have metal is plated on matrix surface
The material of layer.
The method that described micro-nano needle wimble structure layer 2 is grown on described conducting base 1 is electrodeposition process or chemistry
Sedimentation；The method that described tin solder 3 is grown on described micro-nano needle wimble structure layer 2 is plating, chemical plating or heat
Immersion plating.
The height of described micro-nano needle wimble structure layer 2 is 0.2 μm~50 μm, in electro-deposition or chemical deposition FAXIA, is led to
Cross the parameters such as control additive concentration, sedimentation time, temperature, electric current density to control the height of micro-nano needle wimble structure layer 2；
The height of described micro-nano needle wimble structure layer 2 is not less than a quarter of the height of described tin solder 3.
Described micro-nano needle wimble structure layer 2 can be primary structure or multilevel hierarchy；When the micro-nano needle of the present invention is bored
When structure sheaf 2 is primary structure, micro-nano needle wimble structure layer 2 both can be one-level micron pin wimble structure layer, can be again one-level
Nanoneedle wimble structure layer, but to ensure that the height of micro-nano needle wimble structure layer 2 is 0.2 μm~50 μm and is not less than described tinbase
The a quarter of the height of solder 3；When described micro-nano needle wimble structure layer 2 is multilevel hierarchy, the size of previous level structure
It is bigger than the size of latter level structure, and height is for 0.2 μm~50 μm and height is not less than the height of described tin solder 3
A quarter, described multilevel hierarchy can be that primary structure 4 is first grown in substrate, then raw on the basis of primary structure 4
Long two grades or tertiary structure 5.
The primary structure of described micro-nano needle wimble structure layer 2 is the metal with relatively regular pin taper looks such as Cu or Ni unit
Element；The afterbody structure of described multilevel hierarchy is that Ni, Ag or Au etc. are difficult to be reacted with Sn the unit for generating intermetallic compound
Element.
Described tin solder 3 is pure Sn, Sn-Ag, Sn-Ag-Cu or Sn-Zn.
Embodiment 1
Lead frame C194 copper alloys are selected to be conducting base, to conducting base oil removing 20s, except 40 DEG C of oil temperature, oil removing
Electric current 3ASD (A/dm2), after deionized water is cleaned, with 20% dilute sulfuric acid 20s is cleaned, and then deionized water rinsing is clean；Will
The target substrate for cleaning up is placed in ready plating solution, 55 DEG C of solution temperature, the chemical deposition micron copper on conducting base
Pin 20min, obtains the copper needle construction that length is 5 μm or so.After deionized water cleaning, in being placed in nickel plating pin plating solution, solution temperature
For 50 DEG C, electric current density 1.2ASD, electroplating time is 10min, and the electro-deposition on micron copper pin obtains length for 500nm's or so
The micro- cone secondary structure of nickel nanometer.Pickling is carried out to the micro-nano needle wimble structure for obtaining using 20% dilute sulfuric acid, to remove possibility
Aerial oxide layer is exposed, in being subsequently placed in tin plating electrolyte, bath temperature is 25 DEG C, and electric current density is 1.0ASD, during plating
Between be 20min, tin thickness is 12 μm or so, and electroplated carries out cleaning and dry up to tin layers.
Embodiment 2
Selection rustless steel is conducting base, to conducting base oil removing 30s, except 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 rinsing is clean；It is placed in nickel plating pin plating solution
In, solution temperature is 50 DEG C, electric current density 1.0ASD, and electrodeposition time is 20min, and electro-deposition obtains length for 700nm or so
Nickel nanocone structures.Pickling is carried out to the micro-nano needle wimble structure for obtaining using 20% dilute sulfuric acid, to remove possible exposure
Aerial oxide layer, in being subsequently placed in tin plating electrolyte, bath temperature is 25 DEG C, and electric current density is 1.2ASD, and electroplating time is
5min, tin thickness is 2 μm or so, and electroplated carries out cleaning and dry up to tin layers.
Embodiment 3
The Cr/Cu Seed Layers for first sputtering one layer of 50/500nm based on semiconductor silicon on silicon substrate are selected, with 20%
Dilute sulfuric acid cleans 20s, and then deionized water rinsing is clean；In being placed in nickel plating pin plating solution, solution temperature is 50 DEG C, electric current density
1.0ASD, electrodeposition time is 20min, and electro-deposition obtains length for the nickel nanocone structures of 700nm or so.Using 20% it is dilute
Sulphuric acid carries out pickling to the micro-nano needle wimble structure for obtaining, and to remove aerial oxide layer may be exposed, and is subsequently placed in plating
In tin liquor, bath temperature is 25 DEG C, and electric current density is 1.2ASD, and electroplating time is 5min, and tin thickness is 2 μm or so, plating
It is complete cleaning is carried out to tin layers to dry up.
In order to evaluate the effect for suppressing growth of tin crystal whisker using micro-nano obtained in the inventive method-stannum composite deposite, this
Invention is tested by the following method：Accelerate growth of tin crystal whisker using indentation test, in micro-nano obtained in the present invention-stannum
The ceramic bead of an a diameter of 1mm is placed on composite deposite and pure tin coating (matched group) respectively, then on ceramic bead
Apply the constant pressure of 200g, kept for 5 days, humidity is 45~55%, temperature is 20~25 DEG C, stannum can be grown in indentation edge brilliant
Must, by the complexity for counting length, diameter and the quantity of indentation edge tin content to judge coating growth of tin crystal whisker.Table 1
To embodiment 1~3 and single tin coating (matched group) to carry out indentation test to evaluate the difficulty or ease of coating growth of tin crystal whisker respectively
Degree.
Table one
As can be seen from Table I, it is multiple using micro-nano obtained in the inventive method-stannum compared to pure tin coating (matched group)
Close coating to have a significant effect the growth for suppressing tin content, the greatest length of tin content, average length, average diameter sum
Amount declines, and the quantity of average length and tin content especially for tin content has obvious inhibitory action, and the present invention passes through
Micro-nano needle wimble structure layer is first introduced on conducting base, the pressure discharged using micro-nano needle wimble structure layer inside tin coating should
Power, so as to reduce the driving force of tin coating whisker growth, suppresses the formation of tin content.
The conducting base of the present invention is not limited to above deposition the pcb board and copper alloy of metal level, on conducting base
The order and composition of deposition micro-nano needle wimble structure layer can be exchanged, but ensure the pin taper pattern of micro nano structure layer, most
The micro nano structure composition 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, electric current density, sedimentation time can be according to reality
Operation is voluntarily adjusted.Any change and adjustment that those skilled in that art are made within foregoing invention is conceived, belong to this
In the protection domain of application.
Present invention disclosed above preferred embodiment is only intended to help and illustrates the present invention.Preferred embodiment is not detailed
All of details is described, it is only described specific embodiment also not limit the invention.Obviously, according to the content of this specification,
Can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is to preferably explain the present invention
Principle and practical application so that skilled artisan can be best understood by and utilize the present invention.The present invention is only
Limited by claims and its four corner and equivalent.
Claims (10)
1. it is a kind of based on micro-nano needle wimble structure suppress growth of tin crystal whisker method, it is characterised in that comprise the following steps：
(1) select a conducting base, and described conducting base cleaned, after cleaning on described conducting base growth of micro-nano
Rice pin wimble structure layer；
(2) and then to described micro-nano needle wimble structure layer clean, remove surface oxide layer, then in described micro-nano needle
Tin solder is grown on wimble structure layer.
2. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, its feature exists
In described conducting base is the pcb board that copper alloy or deposition have metal level.
3. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, its feature exists
In cleaning to described conducting base described in step (1) includes oil removing and pickling；Step (2) is bored to described micro-nano needle
Structure sheaf carries out cleaning includes pickling.
4. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, its feature exists
In the height of described micro-nano needle wimble structure layer is 0.2 μm~50 μm.
5. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, its feature exists
In described micro-nano needle wimble structure layer is primary structure or multilevel hierarchy.
6. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 5, its feature exists
In when described micro-nano needle wimble structure layer is multilevel hierarchy, the size of previous level structure is bigger than the size of latter level structure.
7. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 5, its feature exists
In the primary structure of described micro-nano needle wimble structure layer is Cu or Ni；The afterbody structure of described multilevel hierarchy be Ni,
Ag or Au.
8. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, its feature exists
In the method that described micro-nano needle wimble structure layer is grown on described conducting base is electrodeposition process or chemical deposition；
The method that described tin solder is grown on described micro-nano needle wimble structure layer is plating, chemical plating or hot-dip.
9. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, its feature exists
In described tin solder is pure Sn, Sn-Ag, Sn-Ag-Cu or Sn-Zn.
10. a kind of method for suppressing growth of tin crystal whisker based on micro-nano needle wimble structure according to claim 1, its feature exists
In the height of described micro-nano needle wimble structure layer is not less than a quarter of the height of described tin solder.
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Cited By (2)
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|---|---|---|---|---|
| CN108914170A (en) * | 2018-06-21 | 2018-11-30 | 上海芮远化学科技有限公司 | The preparation method and electro-plating method of a kind of composite plating solution, composite plating solution |
| CN109722683A (en) * | 2019-01-04 | 2019-05-07 | 中国科学院合肥物质科学研究院 | Gold nano structure and its preparation method and application with cone spiked surface |
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