CN110153592A - A kind of In-Ni system solder and preparation method thereof - Google Patents
A kind of In-Ni system solder and preparation method thereof Download PDFInfo
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- CN110153592A CN110153592A CN201910534201.2A CN201910534201A CN110153592A CN 110153592 A CN110153592 A CN 110153592A CN 201910534201 A CN201910534201 A CN 201910534201A CN 110153592 A CN110153592 A CN 110153592A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3033—Ni as the principal constituent
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Abstract
The invention belongs to technical field of soldering materials, a kind of In-Ni system solder and preparation method thereof is more particularly related to.It is In-xNi composite particles solder that In-Ni system solder of the present invention, which forms general formula by In particle and Ni particle, and wherein X represents the weight percent of the Ni in solder, and the X is 15-75.The present invention has lower fusing point compared to Sn using In, can be realized using TLP interconnection technique and is bonded under lower temperature；In In-Ni system binary alloy phase diagram, the minimum Ni of fusing point3In7Phase fusing point has all reached 409 DEG C；The advantages of realizing low-temperature bonding, high-temperature service.
Description
Technical field
The invention belongs to technical field of soldering materials, a kind of In-Ni system solder and preparation method thereof is more particularly related to.
Background technique
The soldering tech interconnection technique accurate as one, plays more and more important in national defense construction and national economy
Effect, be related to the multiple fields such as Aeronautics and Astronautics, nuclear energy, automobile and electronics, industry exists to the demand of high-temperature electronic device
It is continuously increased, the requirement to soldering is also higher and higher.At the same time, third generation semiconductor (wide bandgap semiconductor, such as SiC and
GaN) have the characteristics that forbidden bandwidth is big, power consumption is low, thermal conductivity is high, component is able to bear higher operating temperature, high
Warm application trend requires to be connected to inside it can continuous service under up to 300 DEG C of adverse circumstances.In order to meet these requirements, 3D
Encapsulation is come into being.The interconnection technique that can be applied to 3D encapsulation field developed at this stage mainly includes metal heat pressing bonding, glues
Mixture bonding and silicon chip bonding, these interconnection techniques are equipped with very big advantage compared to traditional electronic seal, but also have phase
When big limitation, such as bonding temperature is high, thermal mismatching is serious, high temperature resistance is poor.
In order to solve these problems, scientific research personnel proposes for the TLP technology in solder brazing to be applied in solder, this is expected to
Realize the target of " low-temperature bonding, high-temperature service ".Technology is or not low temperature transition liquid-phase (transient liquid phase, TLP)
Only meet the requirement of " low-temperature bonding, high-temperature service " well, it is ensured that the quick and quality of reaction.Currently, both domestic and external
Research is concentrated mainly on bonding technology and encapsulates solder joint tissue change and the life of IMC to the 3D of Ag-In, Cu-In, In-Sn system
Long dynamics, very few for the correlative study of In-Ni system solder, especially bonding technology encapsulates solder joint to In-Ni system 3D
Influence in terms of there is no in-depth study.
However, 156 DEG C of In fusing point, Sn fusing point is 231 DEG C, and lower fusing point not only contributes to be sealed under low-temperature condition
Dress, avoids causing electronic component biggish injury, can also substantially reduce solder joint manufacturing cost.Studies have shown that Sn and In are gathered around
There is identical square crystal structure, the atomic radius of Sn is 145pm, and the atomic radius of In is 156pm.Biggish atom
Radius is more advantageous to In atom and other atom forming cores form new intermetallic compound.
Summary of the invention
The object of the present invention is to provide a kind of low-temperature bonding, the In-Ni system solder of high-temperature service, In has more compared to Sn
Low fusing point can be realized using TLP interconnection technique and be bonded under lower temperature；In In-Ni system binary alloy phase diagram, fusing point is most
Low Ni3In7Phase fusing point has all reached 409 DEG C.
The present invention is achieved through the following technical solutions above-mentioned purpose, a kind of In-Ni system solder, the In-Ni body
It is In-xNi composite particles solder that brazing filler metal, which forms general formula by In particle and Ni particle, and wherein X represents the weight of the Ni in solder
Percentage, the X are 15-75；It such as can be 15wt%, 30wt%, 45wt%, 60wt%, 75wt%.
Preferably, X is 30 in the In-xNi composite particles solder；It is 260 DEG C in bonding temperature, bonding pressure is
Under conditions of 3MPa, bonding time are 90min, with the increase of In content in solder, IMC quantity is gradually decreased in solder joint, and
Black hole is minimum when solder ingredient is In-30Ni；Shear strength first rises as the increase of In content in solder shows
The trend for then declining and tending towards stability rapidly, and reaching peak when solder ingredient is In-30Ni is 7.9MPa.
According to another aspect of the present invention, the present invention provides a kind of preparation methods of In-Ni system solder, including such as
Lower step:
1) preparation of composite soldering powder
By In particle and Ni particle according to weight ratio, In-xNi mixed-powder is allotted；Secondly powder is sufficiently mixed
Colophony type scaling powder is added after even, In-xNi hybrid particles solder paste is obtained after being stirred；The colophony type helps
The weight ratio of solder flux and In-xNi mixed-powder is 1:9；
2) surface of test piece is handled
It selects red copper as baseplate material, is polished using sand paper is carried out the surface of red copper baseplate material, to needs
The red copper substrate material charge level being brazed is polished with W1.5 diamond paste, is disposed and is cleaned with absolute alcohol and cold
Wind is dry
3) process is coated
The lower red copper for being 12mm × 12mm by the size that In-xNi hybrid particles solder paste is uniformly applied to step 2) processing
Baseplate material, the red copper baseplate material end face polishing that the size by step 2) processing is 10mm × 10mm is used as upper substrate, and upper
Substrate is assembled into sandwich structure sample；In-xNi hybrid particles solder paste coating with a thickness of 30 μm.
4) bond sequence
Sandwich structure sample is placed in wafer bonding machine and is bonded, then it is air-cooled to obtain the final product；The condition of the bonding are as follows:
Bonding temperature is 220 DEG C -300 DEG C, bonding pressure 0.1MPa-5MPa, bonding time 30min-180min.
Preferably, the bonding time of the step 4) bonding is 180min；Under 260 DEG C, the bonding conditions of 3MPa, with
The increase of bonding time, IMC quantity, which shows first to rise, reaches slightly downward trend after maximum value, and maximum value appears in bonding
120min, at this time matrix IMC (Ni3In7) and interface I MC (Cu2In) quantity is most, and the hole in tissue is also minimum, but is bonded
After 180min, matrix IMC quantity is reduced and pore quantity increases；With the extension of bonding time, shear strength first increases and subtracts afterwards
Small, when bonding time is 120min, shear strength is up to 9.24MPa；
Preferably, the bonding pressure of the step 4) bonding is 3MPa；Under 260 DEG C, the bonding conditions of 120min, with
The increase of pressure, matrix IMC (Ni in solder joint tissue3In7) form and high number improve, and reach when pressure is 3MPa compared with
Excellent state, black hole is also minimum in tissue at this time.When bonding pressure reaches 5MPa, matrix IMC in solder joint tissue
(Ni3In7) significant change does not occur for quantity and form, only black region is increased slightly；With the increase of bonding pressure,
Shear strength first increases and then decreases, when bonding pressure is 3MPa, shear strength is up to 9.36MPa.
Preferably, 4) bonding temperature of the described bonding is 260-280 DEG C, further preferably 280 DEG C；?
Under the bonding conditions of 120min, 3MPa, with the increase of bonding temperature, matrix IMC (Ni in solder joint tissue3In7) quantity gradually increases
Reach mostly and at 280 DEG C of temperature maximum, black pore quantity is minimum in tissue at this time.When bonding temperature reaches 300 DEG C, base
There is no variations substantially by body IMC, but generate a large amount of continuous holes because atom diffusion rate is different in interface.With key
The raising of temperature is closed, shear strength first increases and then decreases, when bonding temperature is 260 DEG C and 280 DEG C, shear strength is respectively
9.23MPa and 9.71MPa.
Preferably, 4) bonding conditions of the bonding of the described bonding are bonding time 120min, bonding pressure 3MPa, key
Close 260 DEG C of temperature.
Compared with prior art, the present invention has the advantage that
1) In has lower fusing point compared to Sn, while can be realized using TLP interconnection technique and being bonded under lower temperature, keeps away
Exempt to cause biggish damage to electronic component in bonding process.
2) according to In-Ni binary alloy phase diagram it is found that in all In-Ni phases, the minimum Ni of fusing point3In7Phase fusing point all reaches
It 409 DEG C, is expected to realize and be on active service under the conditions of 400 DEG C.
Detailed description of the invention
Fig. 1 is that solder coats schematic diagram；
Fig. 2 is the metallographic structure figure for the solder joint that the In-XNi of different Ni contents is prepared；
Fig. 3 is the shear strength figure for the solder joint that the In-XNi of different Ni contents is prepared；
Fig. 4 is the metallographic structure figure for the Cu/In-30Ni/Cu solder joint that different bonding times are prepared；
Fig. 5 is the shear strength figure for the Cu/In-30Ni/Cu solder joint that different bonding times are prepared；
Fig. 6 is the Cu/In-30Ni/Cu solder joint metallographic structure obtained under different bonding pressures；
Fig. 7 is the shear strength figure of the Cu/In-30Ni/Cu solder joint obtained under different bonding pressures；
Fig. 8 is the Cu/In-30Ni/Cu solder joint metallographic structure obtained under different bonding temperatures；
Fig. 9 is the shear strength figure of the Cu/In-30Ni/Cu solder joint obtained under different bonding temperatures；
Figure 10 is In-Ni binary alloy phase diagram.
Specific embodiment
In powder used in embodiment and Ni powder particles degree are 1 μm, select red copper as baseplate material, are prepared with wire cutting
Size is respectively that 12mm × 12mm × 4mm and 10mm × 10mm × 4mm size copper sheet is several, and the purity of copper sheet is 99.9%.
Test procedure:
The preparation of composite soldering powder: firstly, by In particle and Ni particle according to In-15Ni, In-30Ni, In-45Ni,
The ratio of In-60Ni, In-75Ni, allot mixed-powder.Secondly the pine that quality is 10% is added after powder being sufficiently mixed uniformly
Odor type scaling powder obtains In-xNi hybrid particles solder paste after being stirred.
Surface of test piece processing: select red copper as baseplate material, preparing size with wire cutting is respectively 12mm × 12mm
× 4mm and 10mm × 10mm × 4mm is big, and small copper block is several.Test must assure that copper block surface finish, it is therefore desirable to cutting
Copper billet after the completion of cutting carries out grinding and polishing, removes surface oxide layer, keeps the smooth and clean of surface.Successively using 240#, 600#,
1000#, 1500# and 2000# sand paper polish to size copper block surface, then choose the face W1.5 being brazed
Diamond paste is polished, and is disposed and is cleaned simultaneously cold wind drying with absolute alcohol.Ensure the uniform of welding point interface and
The specification of test need to control big copper block when grinding with a thickness of 3.925mm, so as to subsequent coated solder thickness at 30 μm.
Bonding test: several big copper blocks with a thickness of 3.925mm ground are put into mold and are coated that (coating is shown
It is intended to as shown in Figure 1).Mold thickness is 3.955mm, and centre is cut into the square hole having a size of 12mm × 12mm, will be big
Copper billet is put into hole.Since copper billet height and mold height are there are height degree is poor, the two fills out solder there are a gap
Be filled in this gap, slided using sheet glass on surface, scrape off excess surface solder, make coat solder with a thickness of 30 μ
m。
The big copper block that coating is completed takes out, and the small copper block ground is placed on solder layer surface, the two heap stacks
After be put into bonder and be bonded, determine a plane principle according to 3 points, be bonded three samples, every time to guarantee solder joint height
The uniformity of degree.Sample is taken out after the completion of bonding, air-cooled label after the completion.
Soldered fitting microscopic structure and mechanics property analysis
1) soldered fitting microscopic structure
The sample that bonding has been completed is cut out into the small strip that width is 2-3mm with wire cutting machine, then uses acrylic powder
End and curing agent are inlayed with mass ratio for 1:1.4 proportion, and inlaying the time is 40min.After the completion of inlaying successively using 180#,
400#, 800#, 1200#, 1500#, 2000# sand paper grind the sample inlayed, in model P-2 after the completion of grinding
Polishing machine on sample is polished, polish liquid level alumina solution.Then existed with GX51Olympus metallographic optical microscopy
The tissue of solder joint is observed under 500 times and 1000 times of multiple, and acquires the metallographic structure image under different multiples each 4.Finally
It is analyzed using X-actINCA150 type energy disperse spectroscopy butt welding point structural constituent.
2) soldered fitting shear strength test
The equipment that this test measurement shear strength is used is electronic universal cupping machine.It is sheared and is tried using clamping mould
Sample, rate of extension 0.02mm/min, the shear strength σ of solder jointcIt is calculated according to following formula (2-1):
In formula:
σc- shear strength (MPa)
F-maximum pull (N)
S-effective area (mm2)
When measuring the shear strength of solder joint under different bonding technologies, at least needs to measure 5 groups of data, cast out maximum therein
Value and minimum value are averaged three intermediate data, the authenticity and reliability of test data are ensured with this.
Example 1 group point is to the tissue of Cu/In-xNi/Cu solder joint and the influence of solder joint shear strength
It is configured to be divided into 5 kinds of solder pastes of In-15Ni, In-30Ni, In-45Ni, In-60Ni, In-75Ni, selectes 260
DEG C, the bonding technology of 3MPa, 90min are bonded.
Fig. 2 is the metallographic structure figure for the solder joint that In-15Ni, In-30Ni, In-45Ni, In-60Ni, In-75Ni are prepared,
Wherein a) In-15Ni in Fig. 2；b)In-30Ni；c)In-45Ni；d)In-60Ni；e)In-75Ni.It can be seen from the figure that In-
The tissue of xNi solder joint is mainly by being located in the middle matrix IMC (grey), the remaining Ni particle (white) of reaction, positioned at boundary
Interface I MC (grey) and hole or unreacted it is complete remaining In (black) composition.
As shown in Fig. 2 a), when Ni content is 15%, formed since the content of In in solder is very high, in solder joint a large amount of
Matrix IMC and interface I MC, Ni particle are analyzed close to reaction completely through EDS, and matrix IMC is Ni3In7, interface I MC is Cu11In9,
White area is Ni, and black region ingredient is In, and illustrating, which has a large amount of In to have neither part nor lot in reaction residue, gets off.With the increasing of Ni content
Add, significant change occurs for solder joint tissue.When Ni content is 30%, as shown in Fig. 2 b), the quantity of IMC is reduced in solder joint, black
Color region area is also reducing, and white Ni particle increases.It is analyzed through EDS, black region complicated component illustrates in solder
In element fundamental reaction is complete, and black region is the hole generated by atom diffusion.When Ni content continues growing, from Fig. 2 c),
D), e) can see, IMC quantity gradually decreases in solder joint, there is a large amount of white Ni particle in tissue, the hole of black is sharply
Increase.This is because In content is very few in solder, after temperature reaches the fusing point of In, the In of liquid is far not enough to fill Ni
The gap of intergranular, with holding time, In and Ni, Cu form compound, finally leave a large amount of hole.
The metallographic structure comparison of solder joint after being bonded by heterogeneity solder is it can be found that only ingredient is In-30Ni
Solder joint tissue in IMC layers it is more uniform continuous, hole is less.
Fig. 3 is the shear strength figure for the solder joint that In-15Ni, In-30Ni, In-45Ni, In-60Ni, In-75Ni are prepared.
The shear strength of Cu/In-30Ni/Cu solder joint under different content is 260 DEG C, when 3MPa, 90min in bonding technology, shearing
Intensity shows the trend for first rising and then declining and tend towards stability rapidly with the increase of In content in solder.Its shear strength
Reaching peak when solder ingredient is In-30Ni is 7.9MPa.
The comprehensive analysis from shear strength, metallographic structure determines In-30Ni for preferably bonding technology parameter.
2 bonding time of embodiment is to the tissue of Cu/In-30Ni/Cu solder joint and the influence of solder joint shear strength
In order to determine reasonable bonding time, chooses the ingredient preferably In-30Ni solder that embodiment 1 is probed into out and carry out key
Close, determine two of them bonding technology parameter: 260 DEG C, 3MPa, bonding time select respectively 5min, 30min, 60min,
120min、180min。
Fig. 4 is the metallographic structure figure for the In-30Ni solder joint that different bonding times are prepared, a) 5min；b)30min；c)
60min；d)120min；e)180min.It can be seen from the figure that the tissue of In-30Ni solder joint is mainly by being located in the middle matrix
IMC (grey), the remaining Ni particle (white) of reaction, interface I MC (grey) and hole or unreacted positioned at boundary are complete remains
Remaining In (black) composition.
As in Fig. 4 a), b) shown in, when bonding time be 5min, 30min when, since bonding time is too short, shape in solder joint
At minute quantity IMC, the Ni unreacted of the In of a large amount of black and white and residue is got off.It is analyzed through EDS, matrix IMC is Ni3In7,
Interface I MC is Cu11In9.With the increase of bonding time, significant change occurs for solder joint tissue.When bonding time increases to successively
During 120min, as in Fig. 4 c), d) shown in, IMC quantity continues to increase in solder joint, the unreacted In and white of black
Ni quantity all in lasting reduction.It is analyzed through EDS, matrix IMC is Ni3In7, interface I MC is then changed into Cu2In.Illustrate with
The extension of bonding time, the In in solder become liquid after reaching fusing point, react to form Ni with Ni3In7Phase, and subsequent
Bonding in persistently grow up.It is reacted with Cu and forms Cu11In9Phase, from Fig. 4 as can be seen that in 5min and 30min, boundary
IMC (Cu at face11In9) quantity is few, after bonding time reaches 60min, with the extension of bonding time, interface
IMC(Cu11In9) quantity does not dramatically increase, this is because forming IMC (Cu in interface11In9) after, Cu11In9Mutually cover
Copper base, hinders the diffusion of copper atom, therefore after being bonded 60min, after interface I MC reaches certain thickness, increases
It gradually stagnates, and has been gradually transformed into Cu when subsequent bonding reaches 120min2In phase.At this point, matrix IMC uniformly continuous, boundary
It is continuous that face IMC is straight, and it is more excellent solder joint tissue that pore quantity is less and Dispersed precipitate.When bonding time continues to extend
When reaching 180min, as shown in Figure 4, because atom diffusion generates a large amount of hole in solder joint.
The diffusion of atom needs the time, it is necessary to assure enough isothermal times can just be such that In, Ni and Cu in solder joint completes
Diffuse to form required intermetallic compound.But bonding time is also unsuitable too long, otherwise will form in solder joint largely because of atom
Diffusion generates hole.It is compared by the metallographic structure of the solder joint of different bonding times it can be found that only bonding time is
In the solder joint tissue of 120min IMC layers it is more uniform continuous, the weak area area of black is also more compared with remaining four kinds of bonding time
It is small.
Fig. 5 is the Cu/In-30Ni/Cu solder joint shear strength figure under different bonding times, from the figure, it can be seen that with
The increase shear strength of bonding time constantly increases, and the 2.85MPa by constantly rises, and finally reaches when being bonded 120min
Maximum value 9.24MPa.Later with the extension of bonding time, shear strength is begun to decline, and is down to after being bonded 180min
8.69MPa。
From the metallographic structure of solder joint, there are a large amount of simple substance In in the solder joint of bonding 5min, 30min, 60min, so that
The shear strength of solder joint at the beginning is not high, and after being bonded 120min, the In reaction in solder joint sufficiently generates enough Cu2In phase and
Ni3In7Phase, IMC quantity increases and is uniformly distributed in solder joint, so that shear strength be made to significantly improve.With the increasing of bonding time
Add, atom is further spread, and hole occurs in solder joint tissue, and in stress, hole is weak area, and crackle is sprouted from here first
It is raw, it then extends, finally makes the premature failure of sample, show as the reduction of shear strength.
From shear strength, comprehensive analysis in metallographic structure and processing technology determines 120min for preferably bonding technology
Parameter.
Influence of 3 bonding pressure of embodiment to Cu/In-30Ni/Cu solder joint tissue and shear strength
In order to determine that reasonable bonding time, the ingredient preferably In-30Ni solder that selection is previously probed into out are bonded,
Determine two of them bonding technology parameter: 260 DEG C, 120min, bonding pressure selects 0.1MPa, 1MPa, 3MPa, 5MPa respectively.
Fig. 6 is the Cu/In-30Ni/Cu solder joint metallographic structure obtained under different bonding pressures, a) 0.1MPa；b)1MPa；c)
3MPa；d)5MPa.It can be seen from the figure that the tissue of solder joint is mainly by being located in the middle matrix IMC (grey), reacting remaining
Ni particle (white), the interface I MC (grey) positioned at boundary and hole (black) composition.
Some researches show that the increase of pressure can be such that weld pads intensity improves, (Wang Haidong pressure is in TLP welding process
Effect Lanzhou University of Science & Technology master thesis, 2011).But pressure cannot infinitely increase, it is excessive just at pressure
Weldering rather than Diffusion Welding.When preparing solder paste, due to inevitably existing between particle using solid powder
Gap, after temperature rises to the fusing point of In, In elements melt is wrapped in Ni since capillarity fills Ni void among particles
Gradually isothermal solidification forms IMC around particle and in subsequent insulating process, so hole will necessarily be generated.Therefore, in key
Applying pressure when conjunction exactly is to reduce and reduce hole finally to meet requirement so that solder joint tissue is finer and close.
As shown in Fig. 6 a), when bonding pressure is 0.1MPa, the IMC in solder joint is separated from each other, and dispersion exists, and is not had
The entirety of a continuous uniform is formed, necessarily will affect the service performance of solder joint.Simultaneously there is also not of uniform size in tissue, and
Continuous hole, these holes be the germinating of crackle and extension channel.With the increase of bonding pressure, from Fig. 6 b), c)
In it can be seen that, matrix IMC (Ni3In7) and interface I MC (Cu2In) all become continuous uniform, form an entirety.And hole
Quantity is persistently reduced, and is only existed on a small quantity when bonding pressure is 3MPa, and no longer continuous, and is dispersed in solder joint tissue,
Greatly reduce harm brought by hole.However when bonding pressure reaches 5MPa, as shown in Fig. 6 d), in solder joint tissue
Matrix IMC (Ni3In7) significant change does not occur for quantity and form, but continuous black lines occurs in interface, this
Black lines are to cause the IMC of interface to grow since pressure is excessive defect occur.
By the metallographic structure comparison of the solder joints of different bonding pressures it can be found that the only bonding pressure solder joint that is 3MPa
Its organize in IMC layer it is more uniform continuously, the quantity of black hole is also less compared with its excess-three kind bonding pressure.
Fig. 7 is the Cu/In-30Ni/Cu solder joint shear strength figure under different bonding pressures, from the figure, it can be seen that with
The increase shear strength of bonding time constantly increases.6.3MPa constantly rises by, finally reaches when bonding pressure is 3MPa
To maximum value 9.36MPa.Later with the increase of bonding pressure, shear strength is begun to decline, and when bonding pressure is 5MPa, is cut
Shearing stress is down to 6.38MPa.
Shear strength variation main cause is the change of tissue.From the metallographic structure of solder joint, bonding pressure is
There are a large amount of holes in 0.1MPa solder joint, so that the shear strength of solder joint at the beginning is not high, when bonding pressure is 3MPa, in solder joint
IMC form and high number improve, so that shear strength be made to significantly improve.However, continuing growing with bonding time, pressure
It is excessive, so that micro-flaw is produced between interface area and copper base, during mechanics shearing, the extension of crackle stress, most
Make the premature failure of sample eventually, shows as the reduction of shear strength.
From shear strength, comprehensive analysis in metallographic structure and processing technology determines 3MPa for preferably bonding technology ginseng
Number.
Influence of 4 bonding temperature of embodiment to Cu/In-30Ni/Cu solder joint tissue and shear strength
In order to determine that reasonable bonding temperature, the ingredient preferably In-30Ni solder that selection is previously probed into out are bonded,
Determine two of them bonding technology parameter: 120min, 3MPa, bonding temperature select respectively 220 DEG C, 240 DEG C, 260 DEG C, 280 DEG C,
300℃。
Fig. 8 be different bonding temperatures under Cu/In-30Ni/Cu solder joint metallographic structure figure, a) 220 DEG C；b)240℃；c)
260℃；d)280℃；e)300℃.It can be seen from the figure that the tissue of In-30Ni solder joint is mainly by being located in the middle matrix IMC
(grey) reacts remaining Ni particle (white), positioned at the complete remaining In of the interface I MC (grey) and hole or unreacted on boundary
(black) composition.
Temperature is different, and the diffusion rate of atom is different, and it is also variant to be formed by tissue.The selection of weld heating temperature is answered
Guarantee to obtain best welding quality within the short time, reaches complete metallurgical bonding.As in Fig. 8 a), b) shown in, work as bonding
When temperature is 220 DEG C, 240 DEG C, since bonding temperature is lower, IMC tissue is not uniform enough, continuous in solder joint.And in organizing still
There are more continuous black regions, analyze through EDS, and matrix IMC is Ni3In7, interface I MC is Cu2In, black region are enriched with In
Element should be the incomplete In of reaction.With the raising of bonding temperature, significant change occurs for solder joint tissue.
During bonding temperature is increased to 280 DEG C successively, as in Fig. 8 c), d) shown in, IMC form and quantity have
It is obviously improved, organizes more uniform continuous.Also area reduces black region, is distributed also more disperse.It is analyzed through EDS, matrix
IMC is Ni3In7, interface I MC is Cu2In, black region element is complicated, is to allow existing unavoidable hole in solder joint.
When bonding temperature reaches 300 DEG C, as shown in Fig. 8 e), matrix IMC is substantially there is no changing, but its interface
There is coarse continuous blocky black region in the IMC at place, this is because bonding temperature is excessively high, the Cu atom diffusion in copper base adds
Fastly, a large amount of continuous holes are generated in interface.
By the metallographic structure comparison of the solder joint under different bonding temperatures it can be found that only bonding temperature is 280 DEG C
In the tissue of solder joint IMC layers it is more uniform continuous, the quantity of black hole is also less compared with its excess-three kind bonding pressure.
Fig. 9 is influence of the different bonding temperatures to Cu/In-30Ni/Cu solder joint shear strength, from the figure, it can be seen that with
The raising shear strength of bonding temperature constantly increase.6.3MPa constantly rises by, finally when bonding temperature is 280 DEG C
Reach maximum value 9.71MPa.Later with the raising of bonding temperature, shear strength is begun to decline, and is 300 DEG C in bonding temperature
When, shear strength is down to 6.73MPa.
The variation of tissue can cause the change of shear strength.From the metallographic structure of solder joint, bonding temperature be 220 DEG C,
240 DEG C, there are a large amount of residue In in solder joint so that the shear strength of solder joint at the beginning is not high, bonding pressure is 260 DEG C, 280
DEG C, when, In reaction in solder joint more rapidly more sufficiently, generates a large amount of Cu2In phase and Ni3In7Phase, IMC quantity increases in solder joint
Add, so that shear strength be made to significantly improve.However, continuing to increase with bonding temperature, temperature is excessively high, and atom diffusion rate adds
Fastly, the formation for greatly facilitating hole, during mechanical test, so that the premature failure of sample, shows as shear strength
Reduction.
From shear strength, comprehensive analysis in metallographic structure and processing technology, although shearing is strong when bonding temperature is 280 DEG C
Degree is up to 9.71MPa, but shear strength is 9.23MPa when bonding temperature is 260 DEG C.Intensity is close, and temperature but differs 20 DEG C,
It is thus determined that 260 DEG C are preferably bonding technology parameter.
Figure 10 is In-Ni binary alloy phase diagram, in all In-Ni phases, Ni3In7The fusing point of phase is minimum, but also reaches
409 DEG C, it can satisfy the condition used under 300 DEG C of high temperature.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (7)
1. a kind of In-Ni system solder, it is characterised in that: the In-Ni system solder forms general formula by In particle and Ni particle
For In-xNi composite particles solder, wherein X represents the weight percent of the Ni in solder, and the X is 15-75.
2. a kind of In-Ni system solder described in claim 1, it is characterised in that: X is in the In-xNi composite particles solder
30。
3. a kind of preparation method of In-Ni system solder described in claim 1, it is characterised in that:
1) preparation of composite soldering powder
By In particle and Ni particle according to weight ratio, In-xNi mixed-powder is allotted, colophony type is added after mixing and helps weldering
Agent obtains In-xNi hybrid particles solder paste after mixing evenly；The weight of the colophony type scaling powder and In-xNi mixed-powder
Than for 1:9；
2) surface of test piece is handled
It selects red copper to be used as baseplate material, is polished using progress sand paper the surface of red copper baseplate material, to needing to carry out
The red copper substrate material charge level of soldering is polished with W1.5 diamond paste, is disposed and is cleaned with absolute alcohol and cold wind is blown
It is dry；
3) process is coated
The lower red copper substrate for being 12mm × 12mm by the size that In-xNi hybrid particles solder paste is uniformly applied to step 2) processing
Material, the red copper baseplate material end face polishing that the size by step 2) processing is 10mm × 10mm is used as upper substrate, with upper substrate
It is assembled into sandwich structure sample；
4) bond sequence
Sandwich structure sample is placed in wafer bonding machine and is bonded, then it is air-cooled to obtain the final product；The condition of the bonding are as follows: bonding
Temperature is 220 DEG C -300 DEG C, bonding pressure 0.1MPa-5MPa, bonding time 30min-180min.
4. preparation method according to claim 3, it is characterised in that: the bonding time of the step 4) bonding is
180min。
5. preparation method according to claim 3, it is characterised in that: the bonding pressure of the step 4) bonding is 3MPa.
6. preparation method according to claim 3, it is characterised in that: 4) bonding temperature of the described bonding is 260-
280℃。
7. according to the described in any item preparation methods of claim 3-6, it is characterised in that: 4) the described bonding conditions are bonding
Time 120min, bonding pressure 3MPa, 260 DEG C of bonding temperature.
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| CN113070602A (en) * | 2021-04-12 | 2021-07-06 | 常熟理工学院 | In-Ag composite solder with high mechanical property and preparation method thereof |
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