CN108061737A - A kind of preparation method of the electron backscatter diffraction sample of tin-based solder interconnection solder joint - Google Patents

A kind of preparation method of the electron backscatter diffraction sample of tin-based solder interconnection solder joint Download PDF

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Publication number
CN108061737A
CN108061737A CN201711276253.1A CN201711276253A CN108061737A CN 108061737 A CN108061737 A CN 108061737A CN 201711276253 A CN201711276253 A CN 201711276253A CN 108061737 A CN108061737 A CN 108061737A
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China
Prior art keywords
polishing
sample
solder joint
tin
solder
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CN201711276253.1A
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Chinese (zh)
Inventor
郭福
王雁
谭士海
马立民
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Beijing University of Technology
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Beijing University of Technology
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Priority to CN201711276253.1A priority Critical patent/CN108061737A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/203Measuring back scattering
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

A kind of preparation method of the electron backscatter diffraction sample of tin-based solder interconnection solder joint belongs to electron microscopic sample preparing technical field.Its processing step is:Corase grinding, rough polishing, second polishing, cleaning.Polishing powder wherein during rough polishing is 0.3~0.5 μm of alpha-aluminium oxide polishing powder, the oxidation silicon suspension that the polishing fluid during second polishing is 0.02~0.05 μm.There is no limit preparation process is simple, no mechanical milling tech, without using instrument, equipment, is limited from place, facility, polishing effect is good for size of the present invention to sample.Tin-based solder solder joint EBSD samples can be readily prepared, clearly EBSD orientation mappings figure can be obtained in scanning electron microscope.

Description

A kind of preparation method of the electron backscatter diffraction sample of tin-based solder interconnection solder joint
Technical field
The invention belongs to electron microscopic sample preparing technical fields, are specifically designed a kind of electronics back of the body of tin-based solder interconnection solder joint and dissipate Penetrate the preparation method of diffraction (EBSD) sample.
Technical background
Forbid having tapered off tin using solder containing lead, electronic product in electronic product by relevant law in the U.S. in 1997 The use of lead solder instead tin base leadless soldering-flux.β-tin has body-centered tetragonal crystal structure, and lattice constant isDue to this crystal structure, β-tin crystal grain is in performances such as mechanics, calorifics, electricity On show different degrees of anisotropy.Research shows at 25 DEG C, the diffusion coefficient of Cu along tin lattice c-axis is 2 × 10-6cm2/ s is it along 500 times of a, b axis.Also, solder joint is usually made of one or three tin crystal grain.Therefore, the electricity of solder joint The reliabilities such as migration, heat fatigue are highly prone to its grain-oriented influence, the influence row of research crystal grain orientation butt welding point reliability For very it is necessary to.
Electron backscatter diffraction (EBSD) technology can observe microscopic appearance, structure and the orientation point of crystalline material simultaneously Cloth, and measurement range is big, precision is high, therefore, is widely used in the analysis of material.EBSD technologies can realize butt welding point The characterization of crystal grain distribution of orientations.But it is high to the sample requirement of test, it is desirable that surface is unstressed (elastic and plastic properties stress), anaerobic Change layer, cleaning, it is smooth, with good electric conductivity.Therefore, find it is a kind of simply and easily for observe the tinbase of EBSD without The preparation method of lead interconnection solder joint is very necessary.
The content of the invention
The object of the present invention is to provide a kind of systems of electron backscatter diffraction (EBSD) sample of tin-based solder interconnection solder joint Preparation Method solves the problems, such as the preparation of tin-based solder interconnection solder joint EBSD samples.Preparation method is simple for process, without using instrument, Equipment limits from place, facility, and polishing effect is good, high yield rate.
In order to achieve the above object, the process step of the invention is as follows:
(1) roughly grind:By tin-based solder solder joint sample 1500#~2000# coated abrasive workings, lubricant is done with water.Along same 3-10min is roughly ground in a direction, and sample surfaces are polished, and remove sample surfaces oxide layer so that sample surfaces cut is consistent.Nothing Need mechanical lapping.It cleans and dries up.With micro- sem observation tin-based solder pad surface, to determine sample surfaces state;
(2) rough polishing:The Alpha-alumina polishing fluid prepared in advance is 1 that is, with mass ratio:5 0.3~0.5 μm of alpha-oxidation The polishing fluid that aluminium polishing powder is uniformly prepared by mixing into deionized water.Alpha-alumina polishing fluid is poured on fibre fluff polishing cloth On, rough polishing 5-10min then is carried out to tin-based solder solder joint sample.Without mechanical polishing.It cleans and dries up.Pass through cross-polarization Sample surfaces after light microscope (PLM) observation is thrown, determine that the cut that sand paper leaves has been removed, and exist without stress.
(3) second polishing:0.02~0.05 μm of silica suspension polishing liquid is poured on synthesis oxide polishing cloth, it is right The tin-based solder solder joint sample that rough polishing is crossed polishes 3-5min again.Without mechanical polishing.It cleans and dries up.It is observed and thrown by PLM Sample surfaces after light, it is ensured that sample surfaces do not have cut, obtain interconnecting solder joint sample for the tinbase of EBSD technologies observation.
In a kind of preparation method of the EBSD samples of tin-based solder interconnection solder joint of the present invention, the solder is tinbase Bianry alloy, ternary alloy three-partalloy or quaternary alloy.Bianry alloy be selected from SnCu series, SnAg series, SnZn series, SnBi series or SnIn series, ternary alloy three-partalloy are selected from SnAgCu series, SnAgBi series or SnAgIn series, quaternary alloy and are selected from SnAgBiIn systems Row lead-free brazing.
In a kind of preparation method of the EBSD samples of tin-based solder interconnection solder joint of the present invention, the welding spot structure is Dock solder joint, ovelapping spot weld or BGA Package (BGA) solder joint.
The present invention a kind of tin-based solder interconnection solder joint EBSD preparation method in, in the step (1), with In the sample of sand paper corase grinding tin-based solder solder joint, micro- sem observation sample surfaces will be used with definite sample surfaces state, Confirmatory sample surface scratch is in the same direction.
In a kind of preparation method of the EBSD samples of tin-based solder interconnection solder joint of the present invention, in the step (2), In rough polishing tin-based solder solder joint sample, sample surfaces will be observed with PLM to determine sample surfaces state, confirmatory sample table The cut that facing sand paper leaves has been removed.
Advantages of the present invention and advantageous effect:
1. in a kind of preparation method of the EBSD samples of tin-based solder interconnection solder joint of the present invention, used during rough polishing 0.3~0.5 μm of alpha-alumina polishing powder, second polishing use 0.02~0.05 μm of silica suspension polishing liquid in the process.
2. the present invention is to sample size, there is no limit.
3. preparation method of the present invention is simple, without using instrument, equipment, being limited from place, facility, polishing effect is good, High yield rate.
Description of the drawings
Fig. 1 be the embodiment of the present invention 1 in Sn3.5Ag solders dock solder joint in scanning electron microscope back scattering as picture;
Fig. 2 is that Sn3.5Ag solders dock solder joint EBSD orientation mapping pictures in the embodiment of the present invention 1;
Fig. 3 is Sn3.0Ag0.5Cu solder BGA solder joints secondary electron image figure in scanning electron microscope in the embodiment of the present invention 2 Piece;
Fig. 4 is Sn3.0Ag0.5Cu solder BGA solder joint EBSD orientation mapping pictures in the embodiment of the present invention 2;
Specific embodiment
Embodiment 1
(1) roughly grind:By Sn3.5Ag solders butt welding point sample 2000# coated abrasive workings, lubricant is done with water.Along same 5min is roughly ground in a direction, and sample surfaces are polished, and remove sample surfaces oxide layer so that sample surfaces cut is consistent.Cleaning And it dries up.Pad surface is docked with micro- sem observation Sn3.5Ag solders, to determine sample surfaces state;
(2) rough polishing:Alpha-alumina polishing powder (the mark pleasure of the Alpha-alumina polishing fluid prepared in advance, i.e. 0.3 μm of 20g MicoPolish II 40-6323-016) polishing fluid that is uniformly prepared by mixing into 100g deionized waters.Alpha-alumina is polished Liquid is poured on fibre fluff polishing cloth (mark pleasureOn 40-7220), then to Sn3.5Ag solders butt welding point sample Carry out rough polishing 5min.It cleans and dries up.Sample surfaces after being thrown by cross-polarization light microscope (PLM) observation, determine that sand paper stays Under cut be removed.
(3) second polishing:By 0.02 μm of silica suspension polishing liquid (mark pleasure220-6380-064) It is poured on synthesis oxide polishing cloth (mark pleasureI 40-7918) on, the Sn3.5Ag solders pair crossed to rough polishing It connects solder joint sample and carries out second polishing 3min.It cleans and dries up.Pass through sample surfaces after PLM observation polishings, it is ensured that sample surfaces There is no cut, obtain the Sn3.5Ag solders butt welding point sample for the observation of EBSD technologies.
Embodiment 2
(1) roughly grind:By Sn3.0Ag0.5Cu solder BGA solder joints sample 1500# coated abrasive workings, lubricant is done with water.Edge 5min is roughly ground in same direction, and sample surfaces are polished, and remove sample surfaces oxide layer so that sample surfaces cut is consistent. It cleans and dries up.With micro- sem observation Sn3.0Ag0.5Cu solders BGA pad surfaces, to determine sample surfaces state;
(2) rough polishing:Alpha-alumina polishing powder (the mark pleasure of the Alpha-alumina polishing fluid prepared in advance, i.e. 0.3 μm of 20g MicoPolish II 40-6323-016) polishing fluid that is uniformly prepared by mixing into 100g deionized waters.Alpha-alumina is polished Liquid is poured on fibre fluff polishing cloth (mark pleasureOn 40-7220), then to Sn3.0Ag0.5Cu solder BGA solder joints Sample carries out rough polishing 5min.It cleans and dries up.Sample surfaces after being thrown by cross-polarization light microscope (PLM) observation, determine sand The cut that paper leaves has been removed.
(3) second polishing:By 0.02 μm of silica suspension polishing liquid (mark pleasure220-6380-064) It is poured on synthesis oxide polishing cloth (mark pleasureI 40-7918) on, the Sn3.0Ag0.5Cu prickers crossed to rough polishing Expect that BGA solder joints sample carries out second polishing 3min.It cleans and dries up.Pass through sample surfaces after PLM observation polishings, it is ensured that sample table Face does not have cut, obtains the Sn3.0Ag0.5Cu solder BGA solder joint samples for the observation of EBSD technologies.

Claims (4)

1. a kind of preparation method of the electron backscatter diffraction sample of tinbase interconnection solder joint, which is characterized in that comprise the following steps:
(1) roughly grind:By tin-based solder solder joint sample 1500#~2000# coated abrasive workings, lubricant is done with water;Along same side To corase grinding 3-10min, sample surfaces are polished, and remove sample surfaces oxide layer so that sample surfaces cut is in the same direction; Without mechanical lapping;It cleans and dries up;With micro- sem observation tin-based solder pad surface, to determine sample surfaces cut along same Direction;
(2) rough polishing:The Alpha-alumina polishing fluid prepared in advance is 1 that is, with mass ratio:5 0.3~0.5 μm of Alpha-alumina is thrown The polishing fluid that light powder is uniformly prepared by mixing into deionized water;Alpha-alumina polishing fluid is poured on fibre fluff polishing cloth, with Rough polishing 5-10min is carried out to tin-based solder solder joint sample afterwards;Without mechanical polishing;It cleans and dries up;It is shown by crossed polarized light Sample surfaces after micro mirror PLM observations are thrown, determine that the cut that sand paper leaves has been removed, and exist without stress;
(3) second polishing:0.02~0.05 μm of silica suspension polishing liquid is poured on synthesis oxide polishing cloth, to rough polishing The tin-based solder solder joint sample crossed polishes 3-5min again;Without mechanical polishing;It cleans and dries up;After PLM observation polishings Sample surfaces, it is ensured that sample surfaces do not have cut, obtain interconnecting solder joint sample for the tinbase of EBSD technologies observation.
2. according to the method for claim 1, which is characterized in that the solder is the bianry alloy of tinbase, ternary alloy three-partalloy or Quaternary alloy.
3. according to the method for claim 2, which is characterized in that bianry alloy is selected from SnCu series, SnAg series, SnZn systems Row, SnBi series or SnIn series, ternary alloy three-partalloy are selected from SnAgCu series, SnAgBi series or SnAgIn series, quaternary alloy Selected from SnAgBiIn series leadless solders.
4. according to the method for claim 1, which is characterized in that welding spot structure is docking solder joint, ovelapping spot weld or ball bar battle array Row encapsulation solder joint.
CN201711276253.1A 2017-12-06 2017-12-06 A kind of preparation method of the electron backscatter diffraction sample of tin-based solder interconnection solder joint Pending CN108061737A (en)

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