CN113376239A - Electrochemical migration testing method and device for power packaging - Google Patents
Electrochemical migration testing method and device for power packaging Download PDFInfo
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Abstract
The invention provides an electrochemical migration testing method and device for power packaging, wherein the testing method comprises the following steps: step S1, printing an electrode pattern to be tested on a substrate by adopting metal nano conductive ink to obtain a sample to be tested; step S2, carrying out plasma surface treatment on the electrode pattern of the sample to be detected; step S3, fixing the sample to be tested on the objective table of the optical microscope, adjusting the focal length and the magnification, and connecting the anode and the cathode of the power supply meter with the electrode of the sample to be tested when a clear and complete image appears; and dripping liquid on a sample to be detected to form a liquid film, starting in-situ observation by adopting in-situ observation equipment while starting a power supply meter to apply voltage, and obtaining an in-situ monitoring picture and a current-voltage change curve of the electrochemical migration process. By adopting the technical scheme of the invention, the method is simple to operate, the period is short, the device is very convenient to build, and the obtained experimental result has good observability and repeatability.
Description
Technical Field
The invention belongs to the technical field of electrochemical migration test in the field of power electronic packaging, and particularly relates to an electrochemical migration test method and device for power packaging.
Background
With continuous innovation of electronic technology and demands for multi-functionalization and portability of electronic devices, electronic components are being developed in the direction of high integration, miniaturization, more pin numbers, lighter and thinner, and the like. The distances among circuit board connectors, chip pins, wires and welding spots in the electronic components are also sharply reduced on the premise that the working voltage in the condition is only a few volts, and the electric field intensity of the working voltage can still reach 100-1000V/cm. Since more than 90% of electronic equipment is used in atmospheric environment, the working environment such as temperature, humidity, dust particles and atmospheric pollutants inevitably affects the electronic equipment, so that electrochemical corrosion and electrochemical migration failure are easy to occur. For example, even 10-6Trace amounts of corrosive gases at graded concentrations can also cause severe corrosion to electronic equipment, resulting in electronic equipment failure.
Electrochemical migration is considered to be an important failure mode of electronic components under the action of electric field and environment. The occurrence of electrochemical migration generally significantly reduces the insulating property of insulating layers of electronic components, even becomes a conductor, and causes a serious short circuit phenomenon, which also causes the components to generate heat, and in serious cases, the components can be burned down, even causing fire accidents. Important causes of electrochemical migration failure are high humidity in the environment, high temperature and electric field strength between the electrodes. Therefore, the method has important practical significance for researching the electrochemical migration behavior among welding spots, conductors or through holes in electronic components or electronic equipment, has important theoretical value and practical significance for establishing the corrosion failure rule of electronic materials under the action of multiple factors and improving the reliability of the electronic components, and can provide theoretical guidance for material selection, design, manufacture, protection, maintenance and the like of electronic circuits and electronic components in electronic equipment systems.
There are two main forms of electrochemical migration, one is dendritic growth: after the metal is dissolved into ions at the anode and migrates to the silver electrode, the ions are reduced into dendrites which continuously grow towards the anode, and when the dendrites contact the anode, the whole loop is short-circuited, so that the electronic component is invalid. The other is the growth of the conductive anode wire: under the condition that both the humidity and the electric field intensity are large, conductive wires continuously growing from the anode to the cathode are formed by conductive metal salt along the interface of the epoxy plate and the glass fiber, and when the conductive wires are contacted with the cathode, the whole loop is in short circuit, so that circuit failure is caused.
However, the existing electrochemical migration test methods such as a wet-heat bias method and a water drop method have the problems that the electrochemical migration is difficult to observe and the migration process is difficult to capture in the test.
Disclosure of Invention
Aiming at the technical problems, the invention discloses an electrochemical migration testing method and device for power packaging, which automatically establishes an electrochemical migration in-situ observation and real-time monitoring platform for electronic materials by taking a thin-liquid membrane method as a research method, and solves the problems of difficulty in electrochemical migration observation, difficulty in capturing the migration process and the like in the test.
In contrast, the technical scheme adopted by the invention is as follows:
an electrochemical migration test method for power packaging, comprising the steps of:
step S1, printing an electrode pattern to be tested on a substrate by adopting metal nano conductive ink to obtain a sample to be tested;
step S2, carrying out plasma surface treatment on the electrode pattern of the sample to be detected;
step S3, fixing the sample to be tested on the objective table of the optical microscope, adjusting proper focal length and magnification, and connecting the anode and cathode of the power supply meter with the electrode of the sample to be tested when clear and complete images appear; and dripping liquid on a sample to be detected to form a liquid film, starting in-situ observation by adopting in-situ observation equipment while starting a power supply meter to apply voltage, and obtaining an in-situ monitoring picture and a current-voltage change curve of the electrochemical migration process. The electrochemical migration condition can be analyzed by in-situ monitoring pictures and current-voltage change curves. The in-situ observation equipment can be a 3D optical microscope or a high-speed camera, and the in-situ monitoring picture shot by the equipment has high definition.
Compared with the traditional electrochemical migration testing method such as a wet-heat bias method and a water drop method, the technical scheme of the thin liquid film method is adopted to form a thin liquid film with a certain thickness on the surface of the sample in advance, and the method has the advantages that the contact area between the sample and the electrolyte can be accurately controlled in the whole experimental process, so that the accuracy of the quantitative analysis of the electrochemical migration process can be improved.
As a further improvement of the present invention, step S1 includes:
step S11, uniformly mixing the metal nano particles with an organic solvent to obtain metal nano conductive ink;
step S12, printing the metal nano conductive ink on a substrate, and after the ink is dried in the air, pre-sintering the printed sample;
and step S13, performing intense pulse light sintering on the sample to finish the preparation of the sample to be detected by electrochemical migration.
As a further improvement of the present invention, in step S11, the metal nanoparticles are one of copper nanoparticles, silver nanoparticles, and silver-coated copper nanoparticles.
As a further improvement of the invention, the organic solvent comprises a mixture of two or more of PVAc, ethyl cellulose, ethyl acetate, 1-2-propanediol, a defoamer, terpineol and DBE.
As a further improvement of the present invention, the mass ratio of the metal nanoparticles to the organic solvent is 7: 1-10: 1.
as a further improvement of the present invention, in step S11, the metal nanoparticles and the organic solvent are vibrated by ultrasound, and then mixed in a paste mixer. Preferably, the ultrasonic oscillation time is 5-10 min, and the rotating speed of the paste mixing machine is 100-1000 r/min; the paste mixing times are 4-6.
As a further improvement of the invention, in step S12, the metal nano conductive ink is printed on the substrate by adopting a screen printing mode, and the mesh number of the screen is 100-300 meshes.
As a further improvement of the invention, the substrate is one of alumina and aluminum nitride ceramic substrates.
As a further improvement of the present invention, in step S12, the metal nano conductive ink is printed in an electrode pattern obtained on a substrate, and the distance between two adjacent conductive patterns is 0.5-3 mm.
As a further improvement of the present invention, in step S12, the parameters of the pre-sintering process are: the heating rate is 1-5 deg.C/min, the heat preservation temperature is 50-100 deg.C, and the heat preservation time is 10-90 min.
As a further improvement of the present invention, in step S13, the parameters of the intense pulse light sintering are: the intense pulse light energy is 0-8.04J/cm, the pulse width is 0-30000 us, and the repetition times are 1-100 times. Preferably, the strong pulse light energy is 0.1-8.04J/cm, and the pulse width is 1-30000 us. Further preferably, the intense pulse light energy is 5-8J/cm, and the pulse width is 1000-.
As a further improvement of the present invention, step S2 further includes fixing the area to be tested with a high temperature adhesive tape, and step S3 dropping a liquid into the area to be tested fixed with the high temperature adhesive tape.
Preferably, the area to be tested is 1-100 mm in area2The square area of (a).
Preferably, the thickness of the high-temperature adhesive tape is 50-200 um.
Preferably, the liquid is one or two mixed solutions of pure water, sodium chloride, sodium sulfate and sodium bromide solution.
As a further improvement of the invention, the atmosphere of the plasma surface treatment is any one of nitrogen, argon and oxygen, the radio frequency time is 1-10 min, and the radio frequency power is 0-200W. Further preferably, the radio frequency power is 0.1-200W.
As a further improvement of the invention, in step S3, the volume of the liquid is 1-100 μ L, and the thickness of the liquid film is 10-100 μm.
As a further improvement of the invention, the applied voltage is 0-30V. Preferably, the applied voltage is 0.1 to 30V. Further preferably, the applied voltage is 2 to 15V.
The invention also discloses a testing device used in the electrochemical migration testing method for power packaging, which comprises a testing platform and a power supply meter, wherein the testing platform is provided with an optical microscope and a substrate, the substrate is positioned on an objective table of the optical microscope, the substrate is provided with a conductive pattern printed by metal nano conductive ink and an electrode used for being connected with the power supply meter, in-situ observation equipment is arranged above an eyepiece of the optical microscope, the substrate is provided with a to-be-tested area which is surrounded by a high-temperature adhesive tape and used for dripping liquid, and a lens of the in-situ observation equipment faces the eyepiece of the optical microscope.
Compared with the prior art, the invention has the beneficial effects that:
firstly, by adopting the technical scheme of the invention, the method is simple to operate, the period is short, the device is very convenient to build, the obtained experimental result has good observability and repeatability, and the built device meets the requirement of the electrochemical migration test of the high-power device and lays a foundation for the subsequent exploration of the electromigration mechanism and failure analysis of the power device. The test platform can be flexibly modified into a high-voltage high-temperature electromigration test platform, so that the electromigration of high-power devices such as automobile electronics, aerospace, power electronic equipment and the like can be simulated and tested, and the electromigration mechanism and failure analysis of the power devices are explored.
Secondly, by adopting the technical scheme of the invention, the sample is pre-sintered before optical sintering, so that the structure of the metal nano-particles after optical sintering is more compact and the porosity is lower, the metal nano-particles can bear higher-strength optical pulse energy, and a better sintering effect is achieved; before electrochemical migration observation, surface plasma treatment is carried out on a sample, so that liquid can be better spread on a substrate, and the non-wetting effect of a high-temperature adhesive tape is utilized, so that the form and the thickness of a liquid film can be accurately controlled, more accurate electrochemical test data can be obtained, and the experiment repeatability and the stability are high.
Thirdly, the power supply meter is combined with the in-situ observation device, the voltage and current changes of the loop can be recorded in real time by the introduction of the power supply meter, and the in-situ observation device can monitor the appearance and the dynamic process of the electrochemical migration product in real time, so that the growth mechanism of the electrochemical product can be further deeply analyzed. Compared with the traditional water drop test method and the wet-heat bias method, the method has the following advantages that: (a) when in-situ observation is carried out, the observation result is clearer, and the sight line cannot be influenced by an aperture generated by liquid level reflection; (b) the high-temperature adhesive tape is introduced during the test, so that the thickness of the thin liquid film is fixed, the position of the thin liquid film is fixed, and the contact area of the thin liquid film and a sample is fixed, so that large errors in different batches of tests can not be caused, and the test has good reproducibility; (c) the whole observation process is simple to operate, short in time and good in result.
Drawings
FIG. 1 is a schematic diagram of an electrochemical migration in-situ observation and real-time monitoring platform constructed in example 1 of the present invention.
FIG. 2 is a graph of current versus time at different electric field strengths during the testing of examples 1-4 of the present invention.
Fig. 3 is an in-situ observation image during the test of example 1 of the present invention, wherein (a) is an in-situ observation image at the beginning of t =0, and (b) - (i) are in-situ observation images of the time t =3s, 8s, 15s, 20s, 23s, 32s, 48s and 60s after the power supply meter is started to apply voltage, respectively.
FIG. 4 is an SEM topography of the product between electrodes at different magnifications and different positions after testing in example 1 of the invention.
The reference numerals include:
1-paper substrate, 2-alumina substrate, 3-optical microscope, 4-optical camera, 5-conductive pattern, 6-electrode, 7-high temperature adhesive tape, 8-power meter, 9-liquid film.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
In view of the incomprehensible prior art, the inventor summarizes specific technical routes of the invention as follows through long-term research and extensive practice: preparing metal nano ink, printing the ink on a substrate by using a screen printer, and performing intense pulse light sintering on a sample after glue discharging and hot pressing treatment. After plasma surface treatment is carried out on the sintered sample, the sample is placed on a self-built electrochemical migration in-situ observation and real-time monitoring platform to complete the observation and recording of electrochemical migration.
The invention is characterized in that a thin liquid membrane method is introduced as an electrochemical migration test method: the thin liquid film method is a method in which two adjacent electrodes to which a constant voltage is applied are connected by a thin liquid film and serve as a site where electrochemical migration occurs. The method is an accelerated experiment method, is commonly used for theoretical research and quantitative research in laboratories, and has the advantages of short experiment period, convenience for in-situ observation and the like. Compared with the traditional water drop test method and the wet-heat bias method, the observation result is clearer, the sight line cannot be influenced by the diaphragm generated by liquid level reflection, the thickness and the position of the thin liquid film are fixed, huge errors in different batches of tests cannot be caused, and the tests have good repeatability. Specifically, the electrochemical migration test method for the power packaging technology comprises the following steps:
the method comprises the following steps: electrochemical migration test sample preparation
Uniformly mixing metal nanoparticles and organic solvents such as ethyl cellulose, ethyl acetate, a defoaming agent, terpineol and the like by ultrasonic oscillation according to a certain mass ratio, and continuously stirring by using a paste mixing machine in the process to obtain the metal nano conductive ink. The metal nanoparticles are one of copper nanoparticles, silver nanoparticles and silver-coated copper nanoparticles. The mass ratio of the nano particles to the organic solvent is 7: 1-10: 1. preferably, the ultrasonic oscillation time is 5-10 min, and the rotating speed of the paste mixing machine is 100-1000 r/min. Preferably, the paste mixing times are 4-6.
Then, printing the metal nano conductive ink on an alumina ceramic substrate by adopting a screen printing mode, and after the ink is naturally dried, performing presintering treatment on a printed sample by using a tube furnace; and finally, performing intense pulse light sintering on the sample by adopting a rapid light sintering system to finish the preparation of the sample to be detected by electrochemical migration.
Wherein the mesh number of the silk screen is 100-300 meshes; the selected substrate is one of alumina and aluminum nitride ceramic substrates; the distance between the adjacent conductive patterns is 0.5-3 mm. The temperature rise rate of the pre-sintering treatment is 0-5 ℃/min, and the temperature is respectively kept at 50-100 ℃ for 10-90 min; the sintering energy of the selected intense pulse light is 0-8.04J/cm, the pulse width is 0-30000 us, and the repetition times are 1-100 times.
Step two: treatment of samples prior to electrochemical migration observation
And (3) taking the obtained metal nano ink pattern as a test electrode, putting the sample into a plasma surface treatment machine for plasma surface treatment, enabling a liquid film to be better spread on the surface of the substrate, fixing a square area with a certain area by using a high-temperature adhesive tape, and further obtaining the liquid film with the thickness consistent with the area, thereby finishing the treatment of the sample before electrochemical migration observation. The gas used for plasma surface treatment is nitrogen, the radio frequency time is 1-10 min, and the radio frequency power is 0-200W; the thickness of the high-temperature adhesive tape is 10-200 mu m. The fixed test area is a square area of 1-100 mm 2.
Step three: construction and observation of electrochemical migration device
Fixing the obtained sample on an objective table of an optical microscope, enabling a lens of in-situ observation equipment to face an eyepiece of the optical microscope, opening in-situ observation software (the in-situ observation software is software connected with the lens, and any software capable of realizing an observation imaging function can be used), adjusting a proper focal length and a proper magnification, connecting the anode and the cathode of a power supply meter with electrodes when a clear and complete image appears on a computer, and finishing the construction of the electrochemical migration device at this moment. And secondly, dripping a certain volume of liquid into the gap reserved in the high-temperature adhesive tape in the second step to form a thin liquid film, starting in-situ observation while starting a power supply meter to apply voltage, and further completing in-situ monitoring of the electrochemical migration process and testing of a current-voltage change curve.
Wherein the liquid is one or two mixed solutions of pure water, sodium chloride, sodium sulfate, sodium bromide and the like; the volume of the liquid drop is controlled to be 1-100 mu L, and the thickness of the liquid film is controlled to be 10-100 mu m; the voltage applied by the power supply meter is 0-30V; the original observation platform is a 3D optical microscope or a high-speed camera.
Specifically, as shown in fig. 1, the testing device used in the electrochemical migration testing method for power packaging includes a testing platform and a power supply meter 8, an optical microscope 3 and a substrate are arranged on the testing platform, the substrate includes a paper substrate 1 and an alumina substrate 2, the alumina substrate 2 is located on the paper substrate 1, the substrate is located on an objective table of the optical microscope 3, a conductive pattern 5 printed by metal nano conductive ink and an electrode 6 used for connecting with the power supply meter 8 are arranged on the alumina substrate 2, an in-situ observation device optical camera 4 is arranged above an eyepiece of the optical microscope 3, an area to be tested for dropping liquid and surrounded by a high-temperature adhesive tape 7 is arranged on the substrate, and a lens of the in-situ observation device faces the eyepiece of the optical microscope 3. Liquid is dripped into the area to be tested to form a liquid film 9, and then the power supply meter 8 is started to apply voltage to start in-situ observation.
In this embodiment, the metal nano conductive ink is silver-coated copper nano ink, the distance between adjacent conductive patterns is 1mm, and the electrode is conductive copper adhesive and is connected with the conductive patterns; the thickness of the liquid film is 10 μm.
The technical solution of the present invention is further described below with reference to several examples.
Example 1
(1) Mixing metal nanoparticles with an organic solvent (ethyl cellulose, ethyl acetate, a defoaming agent, terpineol and the like in a mass ratio of 1: 1: 2: 1: 10) in a mass ratio of 6: 4, uniformly mixing, wherein ultrasonic oscillation is adopted for 5 min during mixing, the rotating speed of a paste mixing machine is 700 r/min, and the repetition frequency is 5 times, so that the metal nano conductive ink is obtained; then, printing metal nano conductive ink on an alumina ceramic substrate by adopting a 200-mesh silk screen, controlling the electrode spacing to be 0.5 mm, and after the ink is naturally dried, carrying out pre-sintering treatment on a sample by utilizing a tube furnace, wherein the pre-treatment temperature is 50 ℃, and the heating rate is 2 ℃/min; and finally, performing intense pulse light sintering on the sample by adopting a rapid light sintering system, wherein the pulse light sintering parameters are as follows: the pulse energy is 7.0J/cm, the pulse width is 3000 us, the number of repetitions is 1, and the pulse form is a single pulse, so that preparation of the electrochemical migration to-be-detected sample is completed.
（2）Taking the metal nano ink pattern obtained in the step (1) as an electrode, carrying out nitrogen plasma surface treatment on a sample, wherein the radio frequency time is 5 min, the radio frequency power is 200W, so that a liquid film can be better spread on the surface of a substrate, and then fixing the area of a test area by using a high-temperature adhesive tape to be 100 mm2And a uniform liquid film having a thickness of 50 μm was obtained, at which time the treatment of the sample before the electrochemical migration observation was completed.
(3) And (3) fixing the sample obtained in the step (2) on a 3D optical microscope objective table, opening in-situ observation software, adjusting a proper focal length and a proper magnification, connecting the positive electrode and the negative electrode of the power supply meter with the electrodes when a clear and complete image appears on a computer, and completing the construction of the electrochemical migration device. And (3) dripping liquid with the volume of 20 mu L into the gap reserved in the high-temperature adhesive tape in the step (2) to form a thin liquid film, starting a power supply meter with the preset voltage of 2V, and simultaneously starting in-situ observation to further finish in-situ monitoring of the electrochemical migration process and testing of a current-voltage change curve.
Example 2
(1) Mixing metal nanoparticles with an organic solvent (ethyl cellulose, ethyl acetate, a defoaming agent, terpineol and the like in a mass ratio of 1: 1: 2: 1: 10) in a mass ratio of 6: 4, uniformly mixing, wherein ultrasonic oscillation is adopted for 5 min during mixing, the rotating speed of a paste mixing machine is 700 r/min, and the repetition frequency is 5 times, so that the metal nano conductive ink is obtained; then, printing metal nano conductive ink on an alumina ceramic substrate by adopting a 200-mesh silk screen, controlling the electrode spacing to be 0.5 mm, and after the ink is naturally dried, carrying out pre-sintering treatment on a sample by utilizing a tube furnace, wherein the pre-treatment temperature is 50 ℃, and the heating rate is 2 ℃/min; and finally, performing intense pulse light sintering on the sample by adopting a rapid light sintering system, wherein the pulse light sintering parameters are as follows: the pulse energy is 7.0J/cm, the pulse width is 3000 us, the number of repetitions is 1, and the pulse form is a single pulse, so that preparation of the electrochemical migration to-be-detected sample is completed.
(2) Taking the metal nano ink pattern obtained in the step (1) as an electrode, and carrying out nitrogen plasma surface treatment on the sample, wherein the radio frequency time is 5 min, and the radio frequency power is 200W, so that the liquid film can be formedBetter spread on the surface of the substrate, and then fixed with a high-temperature adhesive tape to form a test area with an area of 100 mm2And a uniform liquid film having a thickness of 50 μm was obtained, at which time the treatment of the sample before the electrochemical migration observation was completed.
(3) And (3) fixing the sample obtained in the step (2) on a 3D optical microscope objective table, opening in-situ observation software, adjusting a proper focal length and a proper magnification, connecting the positive electrode and the negative electrode of the power supply meter with the electrodes when a clear and complete image appears on a computer, and completing the construction of the electrochemical migration device. And (3) dripping liquid with the volume of 20 mu L into the gap reserved in the high-temperature adhesive tape in the step (2) to form a thin liquid film, starting a power supply meter with the preset voltage of 5V, and simultaneously starting in-situ observation to further finish in-situ monitoring of the electrochemical migration process and testing of a current-voltage change curve.
Example 3
(1) Mixing metal nanoparticles with an organic solvent (ethyl cellulose, ethyl acetate, a defoaming agent, terpineol and the like in a mass ratio of 1: 1: 2: 1: 10) in a mass ratio of 6: 4, uniformly mixing, wherein ultrasonic oscillation is adopted for 5 min during mixing, the rotating speed of a paste mixing machine is 700 r/min, and the repetition frequency is 5 times, so that the metal nano conductive ink is obtained; then, printing metal nano conductive ink on an alumina ceramic substrate by adopting a 200-mesh silk screen, controlling the electrode spacing to be 0.5 mm, and after the ink is naturally dried, carrying out pre-sintering treatment on a sample by utilizing a tube furnace, wherein the pre-treatment temperature is 50 ℃, and the heating rate is 2 ℃/min; and finally, performing intense pulse light sintering on the sample by adopting a rapid light sintering system, wherein the pulse light sintering parameters are as follows: the pulse energy is 7.0J/cm, the pulse width is 3000 us, the number of repetitions is 1, and the pulse form is a single pulse, so that preparation of the electrochemical migration to-be-detected sample is completed.
(2) Taking the metal nano ink pattern obtained in the step (1) as an electrode, carrying out nitrogen plasma surface treatment on a sample, wherein the radio frequency time is 5 min, the radio frequency power is 200W, so that a liquid film can be better spread on the surface of a substrate, and then fixing the area of a test area by using a high-temperature adhesive tape to be 100 mm2And further a uniform liquid film having a thickness of 50 μm is obtained, at which point the electrochemical migration is completedTreatment of the samples before observation.
(3) And (3) fixing the sample obtained in the step (2) on a 3D optical microscope objective table, opening in-situ observation software, adjusting a proper focal length and a proper magnification, connecting the positive electrode and the negative electrode of the power supply meter with the electrodes when a clear and complete image appears on a computer, and completing the construction of the electrochemical migration device. And (3) dripping liquid with the volume of 20 mu L into the gap reserved in the high-temperature adhesive tape in the step (2) to form a thin liquid film, starting a power supply meter with the preset voltage of 10V, and simultaneously starting in-situ observation to further finish in-situ monitoring of the electrochemical migration process and testing of a current-voltage change curve.
Example 4
(1) Mixing metal nanoparticles with an organic solvent (ethyl cellulose, ethyl acetate, a defoaming agent, terpineol and the like in a mass ratio of 1: 1: 2: 1: 10) in a mass ratio of 6: 4, uniformly mixing, wherein ultrasonic oscillation is adopted for 5 min during mixing, the rotating speed of a paste mixing machine is 700 r/min, and the repetition frequency is 5 times, so that the metal nano conductive ink is obtained; then, printing metal nano conductive ink on an alumina ceramic substrate by adopting a 200-mesh silk screen, controlling the electrode spacing to be 0.5 mm, and after the ink is naturally dried, carrying out pre-sintering treatment on a sample by utilizing a tube furnace, wherein the pre-treatment temperature is 50 ℃, and the heating rate is 2 ℃/min; and finally, performing intense pulse light sintering on the sample by adopting a rapid light sintering system, wherein the pulse light sintering parameters are as follows: the pulse energy is 7.0J/cm, the pulse width is 3000 us, the number of repetitions is 1, and the pulse form is a single pulse, so that preparation of the electrochemical migration to-be-detected sample is completed.
(2) Taking the metal nano ink pattern obtained in the step (1) as an electrode, carrying out nitrogen plasma surface treatment on a sample, wherein the radio frequency time is 5 min, the radio frequency power is 200W, so that a liquid film can be better spread on the surface of a substrate, and then fixing the area of a test area by using a high-temperature adhesive tape to be 100 mm2And a uniform liquid film having a thickness of 50 μm was obtained, at which time the treatment of the sample before the electrochemical migration observation was completed.
(3) And (3) fixing the sample obtained in the step (2) on a 3D optical microscope objective table, opening in-situ observation software, adjusting a proper focal length and a proper magnification, connecting the positive electrode and the negative electrode of the power supply meter with the electrodes when a clear and complete image appears on a computer, and completing the construction of the electrochemical migration device. And (3) dripping liquid with the volume of 20 mu L into the gap reserved in the high-temperature adhesive tape in the step (2) to form a thin liquid film, starting a power supply meter with the preset voltage of 15V, and simultaneously starting in-situ observation to further finish in-situ monitoring of the electrochemical migration process and testing of a current-voltage change curve.
The current-time curves under different electric field strengths in the test processes of examples 1-4 are shown in fig. 2, the in-situ observation map in the test process of example 1 is shown in fig. 3, and the SEM morphology of the product between the electrodes after the test of example 1 is shown in fig. 4. Therefore, by adopting the technical scheme of the embodiment of the invention, clear observation results can be obtained, the voltage and current changes of the loop can be recorded in real time, the error is small, the operation of the whole observation process is simple, the time is short, the result is accurate, and the experiment repeatability and stability are high.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. An electrochemical migration test method for power packaging, characterized by: which comprises the following steps:
step S1, printing an electrode pattern to be tested on a substrate by adopting metal nano conductive ink to obtain a sample to be tested;
step S2, carrying out plasma surface treatment on the electrode pattern of the sample to be detected;
step S3, fixing the sample to be tested on the objective table of the optical microscope, adjusting the focal length and the magnification, and connecting the anode and the cathode of the power supply meter with the electrode of the sample to be tested when a clear and complete image appears; and dripping liquid on a sample to be detected to form a liquid film, starting in-situ observation by adopting in-situ observation equipment while starting a power supply meter to apply voltage, and obtaining an in-situ monitoring picture and a current-voltage change curve of the electrochemical migration process.
2. The electrochemical migration test method for power packages of claim 1, wherein: step S1 includes:
step S11, uniformly mixing the metal nano particles with an organic solvent to obtain metal nano conductive ink;
step S12, printing the metal nano conductive ink on a substrate, and after the ink is dried in the air, pre-sintering the printed sample;
and step S13, performing intense pulse light sintering on the sample to finish the preparation of the sample to be detected by electrochemical migration.
3. The electrochemical migration test method for power packages of claim 2, wherein: in step S11, the metal nanoparticles are one of copper nanoparticles, silver nanoparticles, and silver-coated copper nanoparticles; the organic solvent comprises a mixture of two or more than two of PVAc, ethyl cellulose, ethyl acetate, 1-2-propylene glycol, a defoaming agent, terpineol and DBE; the mass ratio of the metal nanoparticles to the organic solvent is 7: 1-10: 1.
4. the electrochemical migration test method for a power package of claim 3, wherein: in the step S11, the metal nanoparticles and the organic solvent are vibrated by ultrasound, and then the metal nanoparticles and the organic solvent are mixed in a paste mixing machine, wherein the ultrasonic vibration time is 5-10 min, and the rotation speed of the paste mixing machine is 100-1000 r/min; the paste mixing times are 4-6.
5. The electrochemical migration test method for power packages of claim 2, wherein: in the step S12, printing metal nano conductive ink on a substrate by adopting a screen printing mode, wherein the mesh number of the screen is 100-300 meshes; the substrate is one of an alumina ceramic substrate and an aluminum nitride ceramic substrate.
6. The electrochemical migration test method for a power package of claim 5, wherein: in step S12, the metal nano conductive ink is printed on the substrate to obtain an electrode pattern, and the distance between two adjacent conductive patterns is 0.5-3 mm.
7. The electrochemical migration test method for a power package of claim 6, wherein: in step S12, the parameters of the pre-sintering process are: the heating rate is 1-5 ℃/min, the heat preservation temperature is 50-100 ℃, and the heat preservation time is 10-90 min;
in step S13, the parameters of the intense pulse light sintering are: the intense pulse light energy is 0-8.04J/cm, the pulse width is 0-30000 us, and the repetition times are 1-100 times.
8. The electrochemical migration test method for power packages of claim 2, wherein: step S2 also includes fixing the area to be tested by using a high temperature adhesive tape, and in step S3, dripping liquid into the area to be tested fixed by the high temperature adhesive tape; the area to be tested is 1-100 mm2A square area of (a); the thickness of the high-temperature adhesive tape is 50-200 um; the liquid is one or two mixed solution of pure water, sodium chloride, sodium sulfate and sodium bromide solution; the plasma surface treatment atmosphere is any one of nitrogen, argon and oxygen, the radio frequency time is 1-10 min, and the radio frequency power is 0-200W.
9. The electrochemical migration test method for a power package of claim 8, wherein: in step S3, the volume of the liquid is 1-100 μ L, and the thickness of the liquid film is 10-100 μm; the applied voltage is 0-30V; in step S3, a 3D optical microscope or a high-speed camera is used to take in-situ monitoring pictures.
10. The test device for use in an electrochemical migration test method of a power package of any one of claims 1 to 9, wherein: the testing platform comprises a testing platform and a power supply meter, wherein the testing platform is provided with an optical microscope and a substrate, the substrate is positioned on an objective table of the optical microscope, the substrate is provided with a conductive pattern printed by metal nano conductive ink and an electrode used for being connected with the power supply meter, an in-situ observation device is arranged above an eyepiece of the optical microscope, the substrate is provided with a to-be-tested area which is surrounded by a high-temperature adhesive tape and used for dripping liquid, and a lens of the in-situ observation device faces the eyepiece of the optical microscope.
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