CN116297586A - EBSD sample of packaging substrate and preparation method thereof - Google Patents
EBSD sample of packaging substrate and preparation method thereof Download PDFInfo
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- CN116297586A CN116297586A CN202211599582.0A CN202211599582A CN116297586A CN 116297586 A CN116297586 A CN 116297586A CN 202211599582 A CN202211599582 A CN 202211599582A CN 116297586 A CN116297586 A CN 116297586A
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- 238000005498 polishing Methods 0.000 claims abstract description 113
- 238000000034 method Methods 0.000 claims abstract description 33
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- 238000000227 grinding Methods 0.000 claims description 27
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- 238000005507 spraying Methods 0.000 claims description 14
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- 229910052799 carbon Inorganic materials 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 10
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/20—Investigating 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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/20—Investigating 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
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/20—Investigating 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
- G01N23/203—Measuring back scattering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/053—Investigating materials by wave or particle radiation by diffraction, scatter or reflection back scatter
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/312—Accessories, mechanical or electrical features powder preparation
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Abstract
According to the package substrate EBSD sample and the preparation method thereof, provided by the invention, the mechanical polishing and the electrolytic polishing and the conductive treatment process are combined, and the ion beam pair of the FIB-SEM dual-beam system is utilized to remove the conductive layer on the surface of the region to be tested, so that the integrity of diffraction pattern information of the region to be tested can be ensured, the conductivity of the package substrate EBSD sample can be maintained to a certain extent, and the oxidation degree of the surface of the package substrate EBSD sample is reduced, so that the package substrate EBSD sample with higher EBSD standard rate can be prepared, and the EBSD standard rate can reach 85% -95% or more; the EBSD sample of the packaging substrate prepared by the preparation method has a large testable area, so that all EBSD test analysis information of blind holes in the packaging substrate can be obtained; compared with the single-FIB ion beam cutting method for preparing the EBSD sample of the packaging substrate, the preparation time is short, the production efficiency is high, and the electrolytic polishing solution in the preparation process can be reused, so that the production cost is reduced to a certain extent.
Description
Technical Field
The invention relates to the field of manufacturing of semiconductor integrated circuit packaging substrates, in particular to an EBSD sample of a packaging substrate and a preparation method thereof.
Background
With the trend of low power consumption, high speed, high density and low voltage of chips, the demand for package substrates is increased, and simultaneously, higher requirements are put on the performance and quality of the package substrates, and in the production process of the package substrates, the size of crystal grains and the grain orientations of different layers can influence the performance and quality of the package substrates.
The Electron Back Scattering Diffraction (EBSD) technology is a technology for determining a crystal structure, an orientation and related information based on analysis of an electron beam excited on an inclined sample surface and forming a diffraction chrysanthemum pool band in a scanning electron microscope, so that the information of microstructure morphology, structure, grain size, shape and orientation distribution of any crystal material can be obtained by using the EBSD technology. The principle of the EBSD technique is: scattered electrons generated by the oblique crystal sample are incident by the electron beam to form a diffraction pattern, and the diffraction pattern carries crystal information such as crystal structure, orientation and the like of a sample scanning area and gives absolute crystal orientation with submicron and resolution. However, EBSD techniques are very sensitive to crystal defects, requiring that all surface defects of the test sample must be removed during the preparation process.
In the prior art, the methods for preparing samples by using EBSD are mainly mechanical polishing, vibration polishing, chemical polishing, electrolytic polishing, focused Ion Beam (FIB) polishing, argon ion polishing, and the like. The sample obtained by mechanical polishing has high flatness and high brightness, and can be prepared into a plurality of samples at the same time, but the preparation period is long, scratches are easy to generate on the surface, and meanwhile, the defect of residual stress exists, so that the EBSD standard rate is seriously reduced; the time consumption for preparing the EBSD sample by vibration polishing is long, the sample treatment cost is high, and the method cannot be suitable for magnesium alloy which is easy to corrode; the EBSD sample prepared by chemical polishing has high speed and high efficiency, is suitable for complex parts, but has poor brightness and can generate larger pollution; the equipment used for preparing the EBSD sample by electrolytic polishing is simple, the cost is low, the preparation period is short and no mechanical deformation exists, but the equipment is only applicable to conductive materials; the period of preparing the EBSD sample by Focused Ion Beam (FIB) polishing is long, but shielding parts around a test area need to be removed during preparation, an observable area is small, and equipment cost is very high; the argon ion polishing can obtain a good surface, mechanical damage to a sample is avoided, but experimental parameters are not well mastered, the experimental instrument cost is too high, so that the method cannot be popularized at present, and heat generated by ion bombardment can possibly cause damage to the surface of an EBSD sample, so that the EBSD calibration rate is greatly influenced.
At present, for some invalid package substrate samples, EBSD technical analysis is required to be carried out on the key parts of the package substrate such as the interconnection surfaces of the blind holes, when the EBSD sample of the package substrate is prepared by selecting FIB polishing, the preparation time of 8 hours is required, the area capable of carrying out EBSD test is very small, and the calibration rate after the test is only about 53%; if mechanical polishing is selected to prepare the EBSD sample of the packaging substrate, any EBSD pattern of the packaging substrate cannot be shot, so that it is important to design a preparation method of the EBSD sample of the packaging substrate with specific parameters.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention is directed to providing an EBSD sample with a package substrate and a method for preparing the same, which are used for solving the problems of low production efficiency, small test area of the EBSD sample, and even serious influence on the EBSD calibration rate caused by no diffraction pattern, which are caused by high cost, long preparation time and complex process flow of the EBSD sample with the prior art.
To achieve the above and other related objects, the present invention provides a method for preparing an EBSD sample of a package substrate, the method comprising the steps of:
mechanically grinding and polishing the packaging substrate;
electrolytic polishing is carried out on the packaging substrate after mechanical polishing treatment by utilizing electrolytic polishing solution with components of inorganic acid and organic alcohol;
conducting treatment of metal spraying or carbon spraying on the packaging substrate after electrolytic polishing;
and removing the gold layer or the carbon layer on the surface of the region to be detected by using a FIB-SEM dual-beam system to obtain the EBSD sample of the packaging substrate.
Optionally, the mechanical polishing treatment comprises the steps of cutting the packaging substrate, curing the packaging substrate by using epoxy resin glue, and sequentially carrying out mechanical grinding and mechanical polishing on the packaging substrate, wherein the polishing liquid adopted by the mechanical polishing comprises alumina polishing liquid with the particle size of 0.3 mu m.
Optionally, when mechanically grinding the package substrate, grinding the package substrate by using abrasive paper of 180 mesh, 360 mesh, 600 mesh, 1200 mesh, 2400 mesh and 4000 mesh in sequence, and rotating the package substrate by 90 ° each time the abrasive paper is replaced until the last grinding mark is eliminated.
Optionally, the specific step of mechanical polishing is; the rotating speed is regulated to 100-500 r/min to polish the packaging substrate for the first time, and alumina polishing solution is added in the process of the first polishing; and then the rotating speed is regulated to 100 r/min-300 r/min for secondary polishing until the polished section of the packaging substrate has no scratch and a bright mirror surface appears in the optical microscope.
Optionally, the time of the mechanical polishing is 0.5min-5min.
Optionally, when the electrolytic polishing is performed, the copper sheet is used as a cathode and connected with the cathode of the power supply, the packaging substrate is used as an anode and connected with the anode of the power supply, the electrolyte is continuously stirred in the electrolytic polishing process until bubbles are generated on the surface of the packaging substrate and the surface of the packaging substrate is a bright mirror surface, and the packaging substrate is taken out after the electrolytic polishing is completed, cleaned and dried.
Optionally, parameters of the electropolishing are set as: the voltage is 5V-10V, the current is 0.5A-3A, and the polishing time is 2 s-30 s.
Optionally, the electrolytic polishing solution used for electrolytic polishing is prepared from phosphoric acid: ethanol: isopropyl alcohol: the DI water is mixed to obtain the product, wherein the mass fraction ratio of the DI water to the product is one of 5:5:1:10 or 5.5:4.5:1:8.
Optionally, the method for removing the gold layer or the carbon layer on the surface of the area to be measured by using the FIB-SEM dual-beam system comprises the steps of placing the packaging substrate subjected to the conductive treatment into a horizontal sample stage of a sample bin, vacuumizing the sample bin, rotating the horizontal sample stage by a certain angle, adjusting the ion beam pair of the FIB-SEM dual-beam system and adjusting parameters, so that the gold layer or the carbon layer on the surface of the area to be measured on the packaging substrate is removed.
Optionally, the parameters of the FIB-SEM dual beam system are: the accelerating voltage of the FIB is 10 kV-30 kV; the beam intensity of the FIB is 30 pA-100 pA.
The invention also provides a packaging substrate EBSD sample, which can be prepared by adopting the preparation method of the packaging substrate EBSD sample according to any one of claims 1 to 10.
The package substrate EBSD sample and the preparation method thereof have the following beneficial effects: the preparation method combines mechanical polishing and electrolytic polishing with a conductive treatment process, and removes the conductive layer on the surface of the region to be tested by utilizing the ion beam pair of the FIB-SEM dual-beam system, so that the integrity of diffraction pattern information of the region to be tested can be ensured, the conductivity of the EBSD sample can be maintained to a certain extent, and the oxidation degree of the surface of the EBSD sample is reduced, thereby preparing the EBSD sample of the package substrate with higher EBSD calibration rate, and the EBSD calibration rate can reach 85% -95% or more; the EBSD sample of the packaging substrate prepared by the preparation method has a large testable area, so that all EBSD test analysis information of blind holes in the packaging substrate can be obtained; compared with the single FIB ion beam cutting method for preparing the EBSD sample of the packaging substrate, the preparation time is short, and the production efficiency is high; the electrolytic polishing solution in the preparation process can be reused, so that the production cost is reduced to a certain extent.
Drawings
Fig. 1 shows a flowchart of a method for preparing an EBSD sample of a package substrate according to the present invention.
Fig. 2 is a graph showing the calibration results of EBSD samples of the package substrate according to the first embodiment of the present invention.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The technical solutions provided by the embodiments of the present invention are described in detail below through the drawings and the specific embodiments.
Fig. 1 is a flowchart of a method for preparing an EBSD sample of a package substrate according to the present invention, as shown in fig. 1, the method comprising the steps of:
s1: mechanically grinding and polishing the packaging substrate;
s2: electrolytic polishing is carried out on the packaging substrate after mechanical polishing treatment by utilizing electrolytic polishing solution with components of inorganic acid and organic alcohol;
s3: conducting treatment of metal spraying or carbon spraying on the packaging substrate after electrolytic polishing;
s4: and removing the gold layer or the carbon layer on the surface of the region to be detected by using a FIB-SEM dual-beam system to obtain the EBSD sample of the packaging substrate.
As an example, the specific procedure of step S1 is: cutting the packaging substrate to be detected until the packaging substrate is of a proper size, encapsulating and solidifying the cut packaging substrate, wherein epoxy resin glue can be specifically used, and a gap which cannot be seen by naked eyes is formed at the interface of the solidified packaging substrate and the epoxy resin glue. And after curing is finished, sequentially carrying out mechanical grinding and mechanical polishing on the packaging substrate, wherein the abrasive paper with 180 meshes, 360 meshes, 600 meshes, 1200 meshes, 2400 meshes and 4000 meshes is sequentially used for grinding during mechanical grinding, and the packaging substrate is simultaneously rotated for 90 degrees and then subjected to the next mechanical grinding every time when the abrasive paper is replaced for grinding until the last grinding mark is eliminated. After finishing the mechanical grinding, mechanically polishing the packaging substrate by using a mechanical polishing process, wherein the mechanical polishing comprises the following specific steps: firstly, carrying out primary polishing on the packaging substrate by adjusting the rotating speed to 100-500 r/min, adding alumina polishing solution with the grain diameter of 0.3 mu m in the primary polishing process, preventing the packaging substrate from generating stress concentration phenomenon during polishing, thereby affecting the EBSD calibration rate, and carrying out secondary polishing by adjusting the rotating speed to 100-300 r/min until the polishing section of the packaging substrate has no scratch and presents a bright mirror surface during observation by an optical microscope, wherein the mechanical polishing time is 0.5-5 min, and the mechanical polishing time can be specifically set according to actual needs.
As an example, the specific procedure of step S2 is: add phosphoric acid to the beaker: ethanol: isopropyl alcohol: an electrolytic polishing solution with the mass fraction ratio of DI water being 5:5:1:10 or 5.5:4.5:1:8, wherein the error of the electrolytic polishing solution is kept not to exceed 5% of the respective mass when the mass fraction of each component is measured; placing the beaker on a magnetic stirrer to ensure that the electrolytic polishing solution can be continuously stirred in the electrolytic polishing process, so that the flow of the electrolytic polishing solution can be promoted, the ion diffusion in a polishing area and the replenishment of the electrolytic polishing solution are ensured, and spots on the surface caused by uneven polishing are avoided; then, the copper sheet is placed in a beaker and connected with a power supply negative electrode, the copper sheet is used as a cathode in electrolysis, a packaging substrate after mechanical polishing is placed in the beaker and connected with a power supply positive electrode, the packaging substrate after mechanical polishing is used as an anode in electrolysis, polishing voltage, current and time in the electrolytic polishing process can directly influence the polishing quality of a sample, therefore, the voltage between the cathode and the anode is 5V-10V, the current is 0.5A-3A, the polishing time is 2 s-30 s, if the current range is exceeded or the polishing time is too long, the sample is easy to be corroded, and if the current range is lower than or the polishing time is too short, a stress layer of the sample cannot be effectively removed, so that the EBSD (electronic component standard) rate of the sample can be seriously influenced. In addition, electropolishing of the sample occurs after mechanical polishing to prevent the effects of scratches on the EBSD calibration rate of the sample.
Optionally, the electrolytic polishing process is continued until bubbles are generated on the surface of the package substrate and the surface of the area to be tested on the package substrate presents a bright mirror surface under an optical microscope, and then the package substrate is taken out of the electrolytic polishing solution and is rapidly cleaned and dried, so that the package substrate after the electrolytic polishing is completed is obtained.
As an example, the specific procedure of step S3 is: because the sample is required to be subjected to conductive treatment when the sample is analyzed by using a Scanning Electron Microscope (SEM), the electrolytic polished packaging substrate is subjected to metal spraying or carbon spraying so as to ensure that the sample can conduct electricity, oxidation of the surface of the packaging substrate can be avoided after the metal spraying or carbon spraying, and therefore, the influence on the EBSD calibration rate of the packaging substrate is reduced.
As an example, the specific procedure of step S4 is: placing the encapsulated substrate subjected to conductive treatment on a horizontal sample stage of a sample bin of an SEM after the conductive adhesive is adhered to the encapsulated substrate, vacuumizing the sample bin, opening an ion beam of a FIB-SEM dual-beam system after the vacuum degree reaches a certain value, adjusting parameters to be acceleration voltage 10 kV-30 kV and beam intensity 30 pA-100 pA, rotating the horizontal sample stage by a certain angle, and adjusting the horizontal sample stage to the position of a region to be detected on the encapsulated substrate, thereby removing a gold layer or a carbon layer on the surface of the region to be detected, and finally obtaining the encapsulated substrate EBSD sample meeting the EBSD technical test requirement.
Optionally, after the EBSD sample of the packaging substrate meeting the requirements is taken out from the horizontal bin, the EBSD sample is placed on a sample stage of 45 degrees, the angle of the sample stage is adjusted to 70 degrees, and a voltage of 30kV is set, so as to complete the test and analysis of the area to be tested.
Example 1
Specifically, cutting the packaging substrate to a proper size, filling epoxy resin glue into the cut packaging substrate for curing, and after curing, mechanically grinding the packaging substrate by using abrasive paper of 180 meshes, 360 meshes, 600 meshes, 1200 meshes, 2400 meshes and 4000 meshes in sequence, wherein the packaging substrate is rotated for 90 degrees and then mechanically ground for the next time when the abrasive paper is replaced for grinding each time until the last grinding mark is eliminated, and mechanically polishing the packaging substrate by using a mechanical polishing process after the mechanical grinding is finished, wherein the packaging substrate is firstly polished for the first time by rotating for 500r/min, alumina polishing liquid with the grain diameter of 0.3 mu m is added in the process of the first polishing, the time of the first polishing is 30s, the rotating speed is adjusted for 300r/min for the second polishing, and the time of the second polishing is 15s, so that the packaging substrate with the polished section having no scratches and the bright mirror surface characteristics when observed under an optical microscope is obtained.
Specifically, phosphoric acid was added to the beaker: ethanol: isopropyl alcohol: placing a beaker on a magnetic stirrer to ensure that the electrolytic polishing solution can be continuously stirred in the electrolytic polishing process, placing a copper sheet into the beaker and connecting with a power negative electrode, taking the copper sheet as a cathode in electrolysis, placing a packaging substrate after mechanical polishing into the beaker and connecting with a power positive electrode, taking the packaging substrate as an anode in electrolysis, setting the voltage between the cathode and the anode to be 5V, setting the current to be 1.6A, and polishing time to be 5s, taking the packaging substrate out of the electrolytic polishing solution, and rapidly cleaning and drying to finish electrolytic polishing.
Specifically, the packaging substrate after electrolytic polishing is subjected to metal spraying treatment.
Specifically, the packaging substrate subjected to metal spraying treatment is stuck with conductive adhesive and then is placed on a horizontal sample stage of a sample bin of an SEM, the sample bin is vacuumized, an ion beam of the FIB-SEM dual-beam system is opened, parameters of the ion beam are adjusted to be 30kV in voltage and 100pA in current, then the horizontal sample stage is adjusted to the position of a region to be tested on the packaging substrate, a gold layer on the surface of the region to be tested is removed, and finally the packaging substrate EBSD sample meeting the requirements of EBSD technical test is obtained.
And observing an EBSD sample of the packaging substrate by using a field emission scanning electron microscope, wherein the operating voltage is set to be 30kV, and the inclination angle is 70 degrees to perform an EBSD technical test, and the calibration rate reaches 92.55%. The experimental results are shown in FIG. 2.
Example two
Specifically, cutting the packaging substrate to a proper size, filling epoxy resin glue into the cut packaging substrate for curing, and after curing, mechanically grinding the packaging substrate by using abrasive paper of 180 meshes, 360 meshes, 600 meshes, 1200 meshes, 2400 meshes and 4000 meshes in sequence, wherein the packaging substrate is rotated for 90 degrees and then mechanically ground for the next time when the abrasive paper is replaced for grinding each time until the last grinding mark is eliminated, and mechanically polishing the packaging substrate by using a mechanical polishing process after the mechanical grinding is finished, wherein the packaging substrate is firstly polished for the first time by rotating for 250r/min, alumina polishing liquid with the grain diameter of 0.3 mu m is added in the process of the first polishing, the time of the first polishing is 15s, the rotating speed is adjusted for 150r/min for the second polishing, and the time of the second polishing is 30s, so that the packaging substrate with the polished section having no scratches and the bright mirror surface characteristics when observed under an optical microscope is obtained.
Specifically, phosphoric acid was added to the beaker: ethanol: isopropyl alcohol: placing a beaker on a magnetic stirrer to ensure that the electrolytic polishing solution can be continuously stirred in the electrolytic polishing process, placing a copper sheet into the beaker and connecting with a power negative electrode, taking the copper sheet as a cathode in electrolysis, placing a packaging substrate after mechanical polishing into the beaker and connecting with a power positive electrode, taking the packaging substrate as an anode in electrolysis, setting the voltage between the cathode and the anode to be 5V, setting the current to be 2A, and polishing time to be 15s, then taking the packaging substrate out of the electrolytic polishing solution, and rapidly cleaning and drying to finish electrolytic polishing.
Specifically, the packaging substrate after electrolytic polishing is subjected to metal spraying treatment.
Specifically, the packaging substrate subjected to metal spraying treatment is stuck with conductive adhesive and then is placed on a horizontal sample stage of a sample bin of an SEM, the sample bin is vacuumized, an ion beam of the FIB-SEM dual-beam system is opened, parameters of the ion beam are adjusted to be 30kV in voltage and 100pA in current, then the horizontal sample stage is adjusted to the position of a region to be tested, a gold layer on the surface of the region to be tested is removed, and finally the packaging substrate EBSD sample meeting the requirements of EBSD technology test is obtained.
And observing an EBSD sample by using a field emission scanning electron microscope, wherein the operating voltage is set to be 30kV, the inclination angle is 70 degrees, and the EBSD test is performed, and the calibration rate reaches 93.89%.
The package substrate EBSD sample and the preparation method thereof have the following beneficial effects: according to the preparation method, a mechanical grinding polishing process and an electrolytic polishing process are combined, and then an ion beam pair of a fiber-beam-assisted laser microscope (FIB-SEM) double-beam system is utilized to remove a conductive layer on the surface of a region to be tested, so that on one hand, the FIB-SEM double-beam system can accurately position and process a sample, and on the other hand, the FIB is a focused beam, compared with the condition that the ion beam damages the sample, the damage to the sample is low, the lattice morphology and the internal defects of the sample can be observed, so that the integrity of diffraction pattern information of the region to be tested can be ensured, the conductivity of an EBSD sample of the packaging substrate can be maintained to a certain extent, and meanwhile, the oxidation degree of the surface of the EBSD sample of the packaging substrate is reduced, and therefore, the EBSD sample with a higher EBSD standard rate can be up to 85% -95% or more; the EBSD sample of the packaging substrate prepared by the preparation method has a large testable area, so that all EBSD test analysis information of blind holes in the packaging substrate can be obtained; compared with the single FIB ion beam cutting method for preparing the EBSD sample of the packaging substrate, the preparation time is short, and the production efficiency is high; the electrolytic polishing solution in the preparation process can be reused, so that the production cost is reduced to a certain extent. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (11)
1. A method for preparing an EBSD sample of a package substrate, the method comprising the steps of:
mechanically grinding and polishing the packaging substrate;
electrolytic polishing is carried out on the packaging substrate after mechanical polishing treatment by utilizing electrolytic polishing solution with components of inorganic acid and organic alcohol;
conducting treatment of metal spraying or carbon spraying on the packaging substrate after electrolytic polishing;
and removing the gold layer or the carbon layer on the surface of the region to be detected by using a FIB-SEM dual-beam system to obtain the EBSD sample of the packaging substrate.
2. The method of manufacturing according to claim 1, characterized in that: the mechanical grinding and polishing process includes cutting the package substrate, curing with epoxy resin adhesive, and mechanical grinding and polishing the package substrate successively.
3. The preparation method according to claim 2, characterized in that: when the packaging substrate is mechanically ground, sand paper with 180 meshes, 360 meshes, 600 meshes, 1200 meshes, 2400 meshes and 4000 meshes is sequentially used for grinding, and the packaging substrate is simultaneously rotated by 90 degrees each time when the sand paper is replaced until the last grinding mark is eliminated.
4. The method of claim 2, wherein the mechanical polishing comprises the steps of; the rotating speed is regulated to 100-500 r/min to polish the packaging substrate for the first time, and alumina polishing solution is added in the process of the first polishing; and then the rotating speed is regulated to 100 r/min-300 r/min for secondary polishing until the polished section of the packaging substrate has no scratch and a bright mirror surface appears in the optical microscope.
5. The preparation method according to claim 2, characterized in that: the time of the mechanical polishing is 0.5min-5min.
6. The method of manufacturing according to claim 1, characterized in that: and when the electrolytic polishing is carried out, the copper sheet is used as a cathode and is connected with the cathode of the power supply, the packaging substrate is used as an anode and is connected with the anode of the power supply, the electrolyte is continuously stirred in the electrolytic polishing process until bubbles are generated on the surface of the packaging substrate and the surface of the packaging substrate is a bright mirror surface, and the packaging substrate is taken out after the electrolytic polishing is finished, cleaned and dried.
7. The method according to claim 1, wherein the parameters of the electropolishing are set as follows: the voltage is 5V-10V, the current is 0.5A-3A, and the polishing time is 2 s-30 s.
8. The method of manufacturing according to claim 1, characterized in that: the electrolytic polishing solution used for electrolytic polishing consists of phosphoric acid: ethanol: isopropyl alcohol: the DI water is mixed to obtain the product, wherein the mass fraction ratio of the DI water to the product is one of 5:5:1:10 or 5.5:4.5:1:8.
9. The method of manufacturing according to claim 1, characterized in that: the method for removing the gold layer or the carbon layer on the surface of the region to be detected by using the FIB-SEM dual-beam system comprises the steps of placing the packaging substrate subjected to conductive treatment into a horizontal sample stage of a sample bin, vacuumizing the sample bin, rotating the horizontal sample stage by a certain angle, adjusting the ion beam pair of the FIB-SEM dual-beam system and adjusting parameters, so that the gold layer or the carbon layer on the surface of the region to be detected on the packaging substrate is removed.
10. The method of claim 9, wherein the parameters of the FIB-SEM dual beam system are: the accelerating voltage of the FIB is 10 kV-30 kV; the beam intensity of the FIB is 30 pA-100 pA.
11. An EBSD sample of a package substrate, characterized in that: the EBSD sample of the package substrate according to any one of claims 1 to 10.
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