CN114646723A - Laminated board internal structure and performance integrity analysis method and application thereof - Google Patents
Laminated board internal structure and performance integrity analysis method and application thereof Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
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- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M7/00—Vibration-testing of structures; Shock-testing of structures
- G01M7/08—Shock-testing
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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- G—PHYSICS
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N3/20—Investigating strength properties of solid materials by application of mechanical stress by applying steady bending forces
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/30—Investigating strength properties of solid materials by application of mechanical stress by applying a single impulsive force, e.g. by falling weight
- G01N3/303—Investigating strength properties of solid materials by application of mechanical stress by applying a single impulsive force, e.g. by falling weight generated only by free-falling weight
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/12—Testing dielectric strength or breakdown voltage ; Testing or monitoring effectiveness or level of insulation, e.g. of a cable or of an apparatus, for example using partial discharge measurements; Electrostatic testing
- G01R31/1227—Testing dielectric strength or breakdown voltage ; Testing or monitoring effectiveness or level of insulation, e.g. of a cable or of an apparatus, for example using partial discharge measurements; Electrostatic testing of components, parts or materials
- G01R31/1263—Testing dielectric strength or breakdown voltage ; Testing or monitoring effectiveness or level of insulation, e.g. of a cable or of an apparatus, for example using partial discharge measurements; Electrostatic testing of components, parts or materials of solid or fluid materials, e.g. insulation films, bulk material; of semiconductors or LV electronic components or parts; of cable, line or wire insulation
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Abstract
The invention provides a method for analyzing the internal structure and performance integrity of a laminated board and application thereof, wherein the method comprises the following steps: and (3) putting a sample to be tested into the medium, heating to a set temperature for sample treatment, treating for a set time, taking out the treated sample, and carrying out test analysis on the medium after the sample treatment to finish the analysis on the internal structure and performance integrity of the laminated board. The method can quickly expose the reliability failure caused by possible detection or undetection in the later stage of the industrial chain of the laminated board, particularly the copper-clad board, the downstream PCB, the terminal test analysis and verification method and the like in advance, and can provide cause and effect relationship analysis and direct technical basis for material improvement, thereby providing an improvement technical idea for the material improvement.
Description
Technical Field
The invention belongs to the technical field of laminate performance detection, and particularly relates to a method for analyzing the internal structure and performance integrity of a laminate and application thereof.
Background
The reliability problems of chemical migration resistance (CAF resistance), pressure resistance, heat resistance and the like in the application of copper clad laminate (copper clad laminate for short) materials are long-standing problems in the technical research of the copper clad laminate, and the reliability of the copper clad laminate is the biggest technical challenge in research and development no matter the traditional FR-4 or the copper clad laminates with high frequency, high speed, high heat conductivity and the like. Although reliability problems may occur in various links from copper clad laminate materials, downstream PCBs to terminal electronic product applications, because various links relate to influences of various factors such as materials, formulas, processes, circuit designs, use environments and the like, how to effectively evaluate the influence of the copper clad laminate materials on the application reliability is a very troublesome task, and related research progresses very little. Along with higher requirements of terminal application on the reliability (including CAF resistance, pressure resistance, heat resistance and the like) of the copper-clad plate material, the related contradiction is more prominent, and breakthrough on a material evaluation detection method is urgently needed. The reliability of the copper clad plate material essentially belongs to the problem of the integrity of the material structure and the performance of the copper clad plate material.
Although the existing copper-clad plate has a large number of analysis and verification methods for reliability, heat resistance, mechanics, processability and the like, and a material verification method for a PCB and a terminal, the copper-clad plate has the condition that a material still fails after being tested and verified in application, and meanwhile, the reason for material failure can not be obtained accurately and quickly, and the problem that whether the internal structure of the copper-clad plate is abnormal or not can not be known is the problem of the integrity of the material structure and performance.
The prior IPC-TM-6502.6.16 PCT method discloses a method for boiling a copper-clad plate in a pressure vessel, keeping the pressure at 15psi for 30+2/-0min, using high-temperature water vapor as a medium for sample treatment, and testing the heat resistance of the sample in soldering tin at 260 ℃.
The existing IPC-TM-6502.6.25 method discloses a test method for manufacturing a special circuit by a copper-clad plate, treating a sample in a high-temperature and high-humidity environment (the temperature is 85 ℃, the humidity is 85% RH), wherein the treatment medium is moisture, and the resistance change between circuits is detected during the treatment. This method is a method of evaluating the tendency of Conductive Anodic Filament (CAF), a phenomenon of electrochemical migration in Printed Wiring Boards (PWB). The conductive anode wire may be composed of a conductive salt, rather than a metal cation. Insufficient insulation for the applied voltage, component failure, and use of the part above the Maximum Operating Temperature (MOT) of the laminate can also result in product failure. This method can be used to evaluate PWB laminate material, PWB design and application parameters, PWB manufacturing process variations, and voltage-fitted connector applications. The method is an evaluation method of the long-term use reliability of the copper-clad plate.
In summary, at present, there is no analysis method or evaluation system capable of systematically evaluating the internal structure and performance integrity of the copper-clad plate, so research and development of an analysis technology for detecting the structure and performance integrity of the copper-clad plate material are needed to establish an effective test analysis method.
Disclosure of Invention
In view of the shortcomings of the prior art, the present invention provides a method for analyzing the internal structure and performance integrity of a laminated board and the application thereof. The method can quickly and early expose the failures of heat-resistant and electric-resistant reliability caused by possible detection or undetected detection in the later stage of the industrial chain such as the laminated board, the copper-clad board, the downstream PCB, the terminal test analysis and verification method and the like, and can provide cause-effect relationship analysis and provide a direct technical basis for material improvement, thereby providing an improvement technical idea for the material improvement.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the present invention provides a method for analyzing the internal structure and performance integrity of a laminate, the method comprising the steps of: and (3) putting a sample to be tested into the medium, heating to a set temperature for sample treatment, treating for a set time, taking out the treated sample, and carrying out test analysis on the medium after the sample treatment to finish the analysis on the internal structure and performance integrity of the laminated board.
The copper-clad plate has copper foil on the surface and optionally contains reinforcing materials (such as glass fiber cloth), fillers, resin, curing agents, auxiliaries, flame retardants and the like inside. Ideally, the copper-clad plate should be a whole molecule which is cross-linked with each other by chemical bonds in the copper-clad plate, but impurities, metal ions, foreign matters, micro bubbles, unreacted resin, unreacted curing agent, reaction by-products, reaction intermediates, inorganic and organic unbound interfaces, phase separation and the like often exist in the copper-clad plate. Most of the internal conditions can not be detected from the outside or can be visually seen from the outside, and a small part of the internal conditions such as micro-bubbles can be detected from the detection, but the source of the internal conditions can not be analyzed, so that the internal structure and the performance integrity of the laminated board are influenced, and further certain performances of the copper-clad plate, certain performances of PCB application or certain performances of terminal application and the like can be influenced.
In the invention, a sample is subjected to temperature rise treatment in a medium, and is subjected to condition treatment with set temperature and time so as to quickly expose the structural and performance integrity problems of the material, the material can possibly release impurities, ions, small molecular substances, soluble components, decomposable structural components and the like after being subjected to medium treatment, meanwhile, the performance of the material can be attenuated and other changes, the failure mode and failure grade of the material can be analyzed and judged by analyzing the types and the content of the substances released into the medium after the sample is treated, whether the performance of the sample in some aspects is defective or not can be judged in advance, and the performance grade of the sample can be evaluated; meanwhile, the failure source can be analyzed according to the type and content of substances released into the medium, and the internal structure of the material can be deduced to obtain the evaluation of the internal structure and performance integrity of the sample; according to the analyzed failure source, a direct technical basis is provided for material improvement, so that an improvement technical idea can be provided for material improvement.
Preferably, before the sample to be measured is placed in the medium, the sample to be measured is subjected to pretreatment, the pretreatment is to drill and mill the sample into a specific size and a specific pattern according to performance analysis requirements, rinse the sample with ultrapure water or ultrasonically clean the sample with ultrapure water and dry the sample, and weigh the weight of each sample. In the invention, the sample pretreatment is carried out to avoid the contamination on the surface of the sample and the interference of the content and the type of the released substances after the subsequent analysis sample treatment.
Preferably, the pre-treatment further comprises etching the copper foil. If the surface of the sample is provided with the copper foil, the copper foil needs to be etched first, so that the base material is completely exposed in the medium, unstable components (such as ions) in the base material can be accelerated to be separated out into the medium, and meanwhile, the interference of the separation of metal ions in the copper foil on the substances released by the subsequent sample can be avoided. If the sample surface is provided with a copper foil and the copper foil is not etched, the precipitation of unstable components in the base material is blocked.
Preferably, before the sample to be measured is placed in the medium, the sample is weighed, so that the weight of the sample is compared before and after the sample is processed.
Preferably, the temperature rise to the set temperature is temperature rise to 40-300 ℃, such as 40 ℃, 50 ℃, 60 ℃, 80 ℃, 100 ℃, 130 ℃, 150 ℃, 180 ℃, 200 ℃, 230 ℃, 250 ℃, 280 ℃ or 300 ℃, and preferably the set temperature range is 60-150 ℃; setting a proper treatment temperature according to the boiling point of the medium; if the temperature is too low, the purpose of quickly exposing the defects of the plate structure and performance integrity is not achieved; if the temperature is too high, the boiling point of the medium can be exceeded, the medium can be volatilized rapidly, and the plate can be directly decomposed and damaged and cannot be analyzed.
Preferably, the treatment setting time is 2 hours (h) or more, for example, 4h, 5h, 6h, 8h, 10h, 12h, 18h, 20h, 24h, etc.; the treatment setting time is preferably 4 hours or more. If the time is too short, it is insufficient to expose the panel structural and performance integrity defects.
Preferably, the medium includes, but is not limited to, any one of water (e.g., ultrapure water), high-pressure steam, an organic solvent, a potassium permanganate solution, an acid solution, an alkali solution, or a combination of at least two thereof. The selection of the medium in the invention mainly considers the medium which can quickly expose the problems of structural defects and performance integrity of the material, and the medium can be selected according to the type of the plate, internal defects, performance stability, concerned performance retention capacity and the like, or one or more of the combination of the mediums can be selected.
Preferably, the organic solvent includes, but is not limited to, one or a mixed solvent of at least two of Dimethylformamide (DMF), Methyl Ethyl Ketone (MEK), cyclohexanone, tetrahydrofuran, toluene, xylene, or chloroform.
Preferably, the acid solution includes, but is not limited to, one or a mixed acid solution of at least two of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid, formic acid, benzoic acid, or permanganic acid.
Preferably, the alkali liquor includes, but is not limited to, one or a mixed alkali liquor of at least two of sodium hydroxide, potassium hydroxide, calcium hydroxide or ammonia water.
Preferably, the method is characterized in that a container is used when a sample to be detected is placed in a medium for sample processing, the container is provided with a sufficient medium backflow device, so that the escape of the medium and the released substances of the sample is avoided in the sample processing process, the accurate qualitative or quantitative analysis is facilitated to obtain the content and the variety of the released substances of the material, the parallel comparison among samples, the samples and the benchmarking samples is facilitated, and the structural and performance integrity level of each material is analyzed.
Preferably, when testing at least two samples, the samples are held in the container at intervals such that each sample substantially contacts the medium.
Preferably, the interval fixing is performed by a clamping groove type device or a U-shaped groove device.
Preferably, the performing of the test analysis on the medium after the sample treatment comprises qualitatively or quantitatively analyzing the sample-released substance in the medium after the sample treatment;
preferably, the medium after the sample is processed is analyzed by any one or a combination of at least two of ion chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, gel chromatography, infrared spectroscopy and nuclear magnetic resonance analysis methods, so as to qualitatively or quantitatively analyze substances released after the sample is processed. The method needs to comprehensively analyze the species and content of substances, the total amount of substances, the species and content of ions and the total amount of ions released by the material.
Preferably, the test analysis of the treated medium is a parallel comparison of the type and/or amount of the sample-released substance in at least two of the treated mediums.
Preferably, the performing of the test analysis on the medium after the sample treatment includes comparing the types and/or contents of the released substances of the samples in the treated medium of the at least two samples subjected to the same treatment temperature and the same treatment time, comparing the types and/or contents of the released substances of the samples in the treated medium of the same sample subjected to the same treatment temperature and the same treatment time, and comparing the types and/or contents of the released substances of the samples in the treated medium of the same sample subjected to the same treatment temperature and the different treatment times.
In the invention, the comparison among samples can analyze the integrity and the quality of the structure and the performance of each material, and the comparison between the conditions that the same material releases substances at the same processing temperature and different processing times and at the same processing time and different processing temperatures can analyze the substance release speed of the material, thereby being beneficial to the analysis of the aging mechanism, the failure mode and the failure mechanism of the material, and further improving and optimizing the material formula.
Preferably, the test analysis of the treated medium comprises the treatment of a known benchmarking sample and a sample to be tested under the same treatment conditions, and the parallel comparative analysis of the type and/or content of the released substances is carried out on the treated medium.
In the invention, a sample with excellent known related performance can be selected as a benchmark sample, the known benchmark sample and a sample to be detected are treated under the same treatment condition, and the treated medium is subjected to parallel comparative analysis of the type and/or content of the released substances. The comparison between the sample and the benchmark sample can analyze the advantages and disadvantages of the structure and performance integrity of each material compared with the benchmark sample, and the comparison between the conditions of the benchmark material releasing substances in the same processing temperature and different processing times and under the same processing time and different processing temperatures can analyze the speed of the substances released into the medium by the benchmark material, thereby being beneficial to the analysis of the aging mechanism, the failure mode and the failure mechanism of the material. This gives an assessment of the integrity of the internal structure and performance of the sample. Meanwhile, the invention can also establish a database of the internal structure and performance integrity of the sample according to the medium analysis data after the benchmark sample is processed, the medium analysis data after the test sample is processed, the analysis failure source, the technical improvement idea and the like, and classify the types, the material contents and the like of the medium precipitated substances in the database, and the medium data of the subsequent test sample can be compared with the existing data in the sample database to evaluate the internal structure and the performance integrity of the sample, and can also obtain the suggestion of the technical idea of material improvement.
Preferably, the method further comprises setting a blank control, namely performing the same treatment on the medium without the sample to be detected as the sample group to be detected, and analyzing the substance type and/or content in the medium after blank treatment. In the present invention, this is subtracted as a blank value for the above sample treatment (deduction of the container, medium and substances introduced in the experimental operation).
Preferably, the method for analyzing the internal structure and performance integrity of the laminated board further comprises the step of carrying out performance test analysis on the processed sample besides analyzing the medium after the sample is processed. The analysis of the processed sample can further verify the conclusion of the medium analysis after the sample is processed, and meanwhile, the test data of the processed sample can reflect the performance level of each material after being processed under severe conditions, thereby being beneficial to perfecting the evaluation of the internal structure and the performance integrity of the plate.
Preferably, the performing of the test analysis on the processed sample includes analyzing the change of the sample performance before and after the processing, the change rate of the sample weight before and after the processing, comparing the change of the sample performance after the same sample is processed at different processing temperatures for the same processing time, comparing the change of the sample performance after the same sample is processed at the same processing temperature for the same processing time, and the like. In the invention, the performance degradation rate before and after the material treatment, the performance degradation rate at the same temperature and different time and the performance degradation rate at different treatment temperatures are analyzed, and the data can show the integrity level of the structure and the performance of each material after the material is treated under the severe condition.
Preferably, the test analysis of the processed sample comprises processing the target sample and the target sample under the same conditions, and performing parallel comparison test and analysis on the property change and weight change rate of the target sample and the target sample. In the invention, the performance changes of the target sample and the benchmark sample before and after treatment, the performance changes at the same temperature and different time and the performance changes at different treatment temperatures are analyzed, and the data can reflect the integrity level of the structure and the performance of each material after the treatment under the severe condition.
Meanwhile, the invention can also add the sample database for the performance test before and after the sample treatment, the failure analysis source, the technical improvement idea and the like, and the subsequently tested sample can be compared with the existing data in the sample database to evaluate the internal structure and the performance integrity of the sample, and can also obtain the suggestion of the technical idea of material improvement.
Preferably, the treated sample is dried sufficiently (for example, dried in the air, baked in an oven at a certain temperature and left to equilibrate at room temperature, etc.) and then weighed to remove the factors affecting the treatment solvent.
Preferably, the performance testing of the sample may be performed by selecting one or at least two of all known copper clad laminate test items, PCB test items, and end-use application test items, including, but not limited to, thermal stress limit (288 ℃), glass transition temperature, drop hammer impact, interlayer adhesion, yellowness value, breakdown strength, dielectric constant and dielectric loss tangent, resistivity, signal delay, passive intermodulation PIM, flexural strength, flexural modulus, thermal decomposition temperature, coefficient of thermal expansion, thermal conductivity, dimensional stability, aging resistance, comparative tracking index, chemical migration resistance (e.g., CAF), and pressure resistance (hi-pot).
As a preferred technical scheme, the method for analyzing the internal structure and the performance integrity of the laminated board, provided by the invention, comprises the following steps of:
s1, pre-treating the sample to be tested, optionally etching copper foil, drilling and milling to a specific size and a specific figure, and washing with ultrapure water and drying; s2, placing the pretreated sample into a container, adding a medium, heating to 40-300 ℃, and treating for more than 2 hours; s3, taking out the processed sample from the container; and S4, performing test analysis on the medium after the sample is processed, and analyzing the type and/or content of the released substances of the sample in the medium.
Preferably, the method for analyzing the internal structure and performance integrity of the laminated board provided by the invention comprises the following steps:
s1, pre-treating a sample to be detected, optionally etching copper foil, drilling and milling into a specific size and a specific pattern, and washing with ultrapure water and drying in the air; s2, placing the pretreated sample into a container, adding a medium, heating to 40-300 ℃, and treating for more than 2 hours; s3, taking out the processed sample from the container; s4, testing and analyzing the medium after the sample is processed, and analyzing the type and/or content of the released substances of the sample in the medium; and S5, fully drying the processed sample, and analyzing the change of the sample performance before and after processing and the change rate of the sample weight before and after processing.
Preferably, the method for analyzing the internal structure and performance integrity of the laminated board provided by the invention comprises the following steps:
s1, pre-treating a sample to be detected, optionally etching copper foil, drilling and milling into a specific size and a specific pattern, and washing with ultrapure water and drying in the air; s2, putting the pretreated sample into a container with a medium reflux device, adding a medium, heating to 40-300 ℃, and treating for more than 2 hours; s3, taking out the processed sample from the container; s4, testing and analyzing the medium after the sample is processed, and analyzing the type and/or content of the released substances of the sample in the medium; and S5, fully drying the processed sample, and analyzing the change of the sample performance before and after processing and the change rate of the sample weight before and after processing.
In another aspect, the present invention provides the use of the method as described above in reliability test analysis of a laminate or copper clad laminate, including reliability analysis of heat resistance, ion migration resistance (e.g., CAF), dielectric strength (hi-pot), and the like.
Compared with the prior art, the invention has the following beneficial effects:
the method for analyzing the internal structure and performance integrity of the laminated board establishes a brand-new structure and performance integrity analysis method and an evaluation model; the method can analyze and prejudge the failure mode and failure grade of the material by analyzing the type and content of substances released into a medium after sample treatment, and evaluate the performance grade of the sample; meanwhile, the failure source can be analyzed according to the type and the content of the substances released into the medium, so that the evaluation of the internal structure and the performance integrity of the sample can be obtained; according to the analyzed failure source, a direct technical basis is provided for material improvement, so that an improvement technical idea can be provided for material improvement.
Drawings
FIG. 1 is a schematic view of a sample processing device;
FIG. 2 is a schematic view of the spacing and fixing of samples in a container;
FIG. 3 is a graph of the change rate of the glass transition temperature of the samples after treatment;
FIG. 4 is a graph of the rate of change of flexural strength of the treated samples;
FIG. 5 is a graph of the rate of change of flexural modulus of the treated samples;
FIG. 6 is a graph showing the dielectric constant and dielectric loss tangent change rate of the treated sample.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1:
s1, taking A, B, C and four copper-clad plate samples of the marker post material, etching to remove the copper foil on the surface, firstly ultrasonically cleaning in ultrapure water for 10min, repeating for 3 times, wearing cotton gloves, taking out and airing. And respectively taking a part of sample to test the initial performance of the four materials, wherein the test performance comprises the following steps: thermal stress limit (288 ℃), glass transition temperature, yellowness number, breakdown strength, dielectric constant and dielectric loss tangent, flexural strength, flexural modulus, thermal decomposition temperature (5% weight loss), drop weight impact, and interlayer adhesion.
According to the selected performance test items, drilling and milling a sample with the size required by the test, ultrasonically cleaning the sample in ultrapure water for 10min and repeating the ultrasonic cleaning for 3 times, wearing cotton gloves, taking out the sample, airing the sample, and weighing the sample.
S2, fixing the samples in a 3L three-port reaction kettle (cleaned in advance) at intervals, adding 950mL of ultrapure water, connecting two condensation pipes for backflow, plugging redundant interfaces of the reaction kettle by plugs, ensuring that substances such as water vapor and the like are completely condensed in the treatment process, and treating at 100 ℃ for 8 hours. The reaction apparatus is shown in FIG. 1, in which the sample intervals are fixed as shown in FIG. 2.
And S3, taking out the sample by using clean tweezers to dry after the treatment is finished, transferring all the treated water into a 1000mL volumetric flask, washing the reaction kettle for multiple times by using about 50mL of ultrapure water, transferring the washing water into the volumetric flask completely, and fixing the volume to 1000 mL.
And (4) performing a blank test without adding a sample according to the steps, and fixing the volume of the water to 1000mL after blank treatment.
And S4, analyzing the concentrations of anions and cations in the water after the sample treatment and the blank treatment by adopting ion chromatography. The anion concentration, cation concentration and total ion content in the aqueous solution after sample treatment (WZ 1-WZ 4 are ions whose species could not be determined temporarily) are shown in Table 1, Table 2 and Table 3 below, respectively.
TABLE 1 anion concentration of aqueous solution after sample treatment
| Sample (I) | F-/ppm | WZ1/ppm | Cl-/ppm | NO2-/ppm | Br/ppm | WZ2/ppm | SO4 2-/ppm |
| Blank space | 0 | 0 | 0.15 | 0 | 0 | 0 | 0.06 |
| A | 0.09 | 0 | 0 | 0.02 | 0.17 | 0.05 | 0 |
| B | 0.10 | 0.10 | 0.00 | 0.00 | 0.05 | 0.05 | 0.00 |
| C | 0.09 | 0.03 | 0.00 | 0 | 0 | 0.03 | 0.00 |
| Mark post | 0.04 | 0.08 | 0.00 | 0 | 0 | 0.04 | 0.00 |
TABLE 2 cation concentration of aqueous solution after sample treatment
| Sample (I) | Li+/ppm | Na+/ppm | K+/ppm | NH4 +/ppm | WZ3/ppm | Mg2+/ppm | Ca2+/ppm | WZ4/ppm |
| Blank space | 0 | 0.25 | 0.14 | 0.00 | 0.01 | 0.05 | 0.18 | 0 |
| A | 0.0138 | 0.25 | 0.00 | 2.46 | 0.29 | 0.35 | 2.45 | 0 |
| B | 0.0144 | 0.16 | 0.01 | 0.00 | 0.00 | 0.13 | 3.24 | 0 |
| C | 0.0131 | 0.04 | 0.00 | 0.00 | 0.00 | 0.09 | 1.52 | 0.008 |
| Marker post | 0.0124 | 0.00 | 0.04 | 0.00 | 0.01 | 0.04 | 0.18 | 0 |
TABLE 3 Total amount of released ions after sample treatment
The minimum ion release from the benchmarking samples was seen from the ion concentration data for each sample, indicating the best structural and performance integrity, followed by C, B, A samples. Four types of materials for comparing release ion data of samplesCa is most released2+And Mg2+The two ions mainly come from filler impurities and glass fiber cloth, which indicates that the two impurities in the filler are unstable or excessive, the bonding force between the filler and resin or other materials is insufficient, the ions in the glass fiber cloth are unstable, and the like, so how to improve the bonding force between the filler and the resin or other materials and how to replace the low-Ca ions in the glass fiber cloth can be considered for improving the internal structural stability of the material2+And Mg2+The filler with ion content, the replacement of the glass fiber cloth and the like.
Preferably, the treated sample is further tested: and S5, fully drying the treated sample (airing, baking for 1h at 105 ℃, taking out and balancing for 3h in a drying oven), testing Tg, yellowness value, puncture strength, Dk/Df, bending strength, bending modulus, drop hammer impact and interlayer adhesive force data, comparing the data with the data of the untreated sample, and analyzing and comparing the change conditions of the performance data between samples and between the sample and a benchmark rod before and after the sample is treated. See tables 4 and 5.
Table 4 sample Performance data 1 before and after treatment
45+ kV NB in table 4 indicates no breakdown at greater than 45 kV.
Table 5 sample pre and post treatment performance data 2
The bending strength in table 5 includes two values, where the first data is warp data and the second data is weft data. The value of the interlayer adhesion was a range of values because the range of the lowest value and the highest value of the adhesion value was recorded as the adhesion value was continuously fluctuated as the test was conducted when the interlayer adhesion test was conducted.
It can be seen from the property change data that the sample has no attenuation change in thermal stress limit (288 ℃) and breakdown strength after treatment, and other properties have certain attenuation. The Tg value of the sample C is improved in the later period of treatment, which shows that the Tg value of the sample C is improved after the Tg value is improved, so that the performance of the sample C is improved after the Tg value is improved, and the performance of other samples are attenuated, and the performance attenuation of the benchmark sample is smaller than that of other samples (see fig. 3, A-1 and A-2 in fig. 3 indicate two parallel test samples of the sample A, and the other B, C samples and the benchmark sample are the same). The performance change data also demonstrates the structural and performance integrity of the material, which is reflected in a lower performance decay rate after the benchmarking sample (structural i.e., higher performance integrity) is processed. Therefore, the structural and performance integrity of the sample can be judged according to the performance decay rate data of the method.
According to the test result of the step S5, the comprehensive performance evaluation of the plate can be given as follows: the benchmarking product C, B, A, which is consistent with the conclusion of the evaluation of the internal structure and performance integrity of the panel given by the test results of step S4.
Example 2:
s1, taking six copper-clad plate samples of A, B, C, D, E and a mark post, etching to remove copper foil on the surface, washing with ultrapure water for 10min, repeating for 3 times, wearing cotton gloves, taking out and airing. And respectively taking a part of samples to test the initial performance of the four materials, wherein the test performance comprises the following steps: thermal stress limit (288 ℃), Tg (DMA method), Dk/Df, flexural strength, flexural modulus, TGA (5% weight loss).
According to the selected performance test items, drilling and milling a sample with the size required by the test, washing with ultrapure water for 10min, repeating for 3 times, wearing cotton gloves, taking out, airing, and weighing the sample.
S2, fixing the samples in a 3L three-port reaction kettle (cleaned in advance) at intervals, adding 450mL of analytically pure toluene, connecting two condensing pipes for backflow, inserting a thermocouple into the middle port of the reaction kettle to detect the temperature of a medium, ensuring that the toluene vapor, the sample release substances and other substances are completely condensed in the treatment process, treating at 90 ℃ for 10 hours, and observing the treatment condition and phenomenon.
And S3, taking out the sample by using clean tweezers to dry after the treatment is finished, transferring all the treated methylbenzene into a 500mL volumetric flask, washing the reaction kettle for multiple times by using about 50mL of analytically pure methylbenzene, and completely transferring the toluene into the volumetric flask to reach the constant volume of 500 mL.
And S4, observing the appearance of the toluene and the plates after the samples are processed, and analyzing the types and the contents of substances released after the samples are processed by adopting equipment such as gel chromatography, a gas mass spectrometer and the like, wherein the types and the contents are shown in tables 6-8.
TABLE 6 toluene/Panel appearance after the end of the treatment
| Sample (I) | Toluene/plate appearance |
| Mark post | The toluene was clear and transparent. |
| A | Toluene insoluble resin is arranged at the bottom of the reaction kettle and is dissolved in MEK |
| B | The bottom of the reaction kettle is filled with filler, and white spots of the plates are obvious. |
| C | The bottom of the reaction kettle is filled with the filler, and white spots of the plate are obvious. |
| D | Slight bubbling of sheet material |
| E | Obvious bubbling of the plate |
TABLE 7 molecular weight of substances contained in toluene after treatment
TABLE 8 composition of substances contained in toluene after treatment
Table 7 analysis of toluene by gel chromatography after sample treatment shows that the molecular weight of organic components is not detected in toluene of the marker post material, and it can be seen that the released substances of the marker post material are less after treatment; whereas the A, B, C, D, E materials all measured substances with a molecular weight of about 60, the B, C sample also measured substances with a molecular weight of about 500. D. The E sample measured about 4000 molecular weight species. It can be seen that 5 materials except the marker post material all released different contents of organic substances with different molecular weights in the treatment, which is consistent with the phenomenon of toluene appearance in table 6. The substances released by the method are analyzed by a gas chromatography-mass spectrometer, and reaction intermediates such as triallyl isocyanurate, benzaldehyde and anisole are contained in the substances. Therefore, the evaluation of the internal performance and the structural integrity of the plate can be given, the evaluation is carried out from the apparent dimensions of the treated methylbenzene and the plate, and the advantages and disadvantages are as follows: the mark post material is more than A and more than B, C and more than D and E, and the quality is evaluated from the dimensionality of the Tg reduction rate of the material: c is greater than B, greater than A, greater than E, greater than mark post and greater than D. From the information, it can be seen that organic substances such as triallyl isocyanurate (raw material for sheet), benzaldehyde (intermediate product), anisole (intermediate product) and the like in the internal structure indicate that triallyl isocyanurate is not completely crosslinked or is not highly crosslinked, and then improvement research needs to be carried out from the perspective of how to increase the crosslinking degree of triallyl isocyanurate and how to reduce benzaldehyde and anisole intermediate products, so as to provide a technical idea for further improving material performance.
S5, fully drying the treated sample (treating in a vacuum oven at 115 ℃ for 4h, taking out and balancing in a room for 3 h). Weighing the treated sample, and testing the performance of the sample by the following steps: thermal stress limit (288 ℃), Tg (DMA method), Dk/Df, flexural strength, flexural modulus, TGA (5% weight loss) and the material after treatment performance degradation rate (performance degradation data before and after treatment/performance data before treatment) for the properties of the untreated samples are compared, see tables 9-11 and fig. 4, 5 and 6.
TABLE 9 weight retention of materials after treatment
TABLE 10 Performance data before and after Material treatment
The flexural strength and flexural modulus in table 10 include two values, the first being warp data and the second being weft data. The thermal stress value of 288 ℃ after the sample E is treated is 15; 10; 10, which represents the test of three samples, the time for plate explosion is 15s, 10s and 10s respectively.
TABLE 11 degradation rate of material after treatment
It can be seen from table 9 that the weight of the samples treated by the benchmarks and A, D, E is larger than that of the samples before treatment, which indicates that the samples absorb toluene after high temperature treatment in toluene, and the toluene penetrates into the interior of the material and is possibly combined with the material molecules. The quality of the samples B and C is slightly reduced compared with the samples before treatment due to the problems of material dissolution, filler shedding and the like. It is apparent from table 6 that toluene is clear and transparent after the flagpole material is treated, so that the problems of obvious material dissolution and shedding and the like occur, and B, C, D, E materials all have the problems of dissolution, shedding, bubbling and the like, and the structural integrity and the performance integrity of the flagpole material are poorer than those of the flagpole sample.
From tables 10-11 and FIGS. 4-6 (A-1, A-2 in FIGS. 4-6 indicate two parallel test specimens of sample A, the other B, C samples and the benchmarking sample are the same) it can be seen that the material was processed: dk performance is improved, which is probably caused by that the material absorbs polar toluene, Df data change is small and is close to instrument errors and is not analyzed; the Tg of the marker post material and other materials is greatly reduced, because the glass transition temperature of the materials is obviously reduced due to the swelling of the materials by toluene; furthermore, the flexural strength of the material is markedly increased by swelling and the flexural modulus is markedly reduced. These information are all due to material structural and performance integrity deficiencies, consistent with the conclusions analyzed in tables 6-8.
The performance test method referred to above is as follows:
anion concentration: IPC-6502.3.28A plate ion contamination test;
cation concentration: IPC-6502.3.28A plate ion contamination test;
total amount of released ions: IPC-6502.3.28A plate ion contamination test;
glass transition temperature: the DMA method defined by IPC-TM-6502.4.24 was used for the measurement.
Thermal stress (288 degree limit): thermal stress of IPC-6502.4.19 laminates;
yellowness value: ASTM E313 calculates yellowness and whiteness values from the color match values measured by the instrument;
breakdown strength: IPC-6502.5.6 laminate breakdown voltage;
dielectric constant and dielectric loss tangent (DK/DF) IPC-TM-6502.5.5;
flexural strength/flexural modulus: IPC-TM-6502.4.4;
drop hammer impact: making a sample into a sample block of 100X100mm, using a 10mm hammer head to freely fall from a certain height to hit the center of the sample block, and measuring the drop mark area on the sample block;
interlayer adhesion: making a sample into a 3mm strip, peeling off a target layer of PP, testing the tension for vertically peeling off the PP by using a tension meter, continuously fluctuating along with the tension value of the test, and recording the tension range of the lowest value and the highest value;
gel chromatography analysis: GB/T21863 gel chromatography;
gas chromatography-mass spectrometry analysis: GB/T38397-2019 coal tar component content determination, gas chromatography-mass spectrometry and thermogravimetric analysis.
TGA thermal decomposition temperature (5% weight loss): IPC-TM 6502.4.24.6 laminate thermal decomposition temperature.
The applicant states that the process of the present invention is illustrated by the above examples, but the present invention is not limited to the above process steps, i.e. it is not meant to imply that the present invention must rely on the above process steps to be carried out. It will be apparent to those skilled in the art that any modification of the present invention, equivalent substitutions of selected materials and additions of auxiliary components, selection of specific modes and the like, which are within the scope and disclosure of the present invention, are contemplated by the present invention.
Claims (10)
1. A method for analyzing the internal structural and performance integrity of a laminate, the method comprising the steps of: and (3) putting a sample to be tested into the medium, heating to a set temperature for sample treatment, treating for a set time, taking out the treated sample, and carrying out test analysis on the medium after the sample treatment to finish the analysis on the internal structure and performance integrity of the laminated board.
2. The method according to claim 1, wherein before the sample to be tested is placed in the medium, the sample to be tested is subjected to pretreatment, wherein the pretreatment comprises the steps of drilling and milling the sample into a specific size and a specific pattern according to performance analysis requirements, washing with ultrapure water or ultrasonically cleaning with ultrapure water, airing and accurately weighing;
preferably, the pre-treatment further comprises etching the copper foil.
3. The method according to claim 1 or 2, wherein the raising to the set temperature is raising to 40-300 ℃;
preferably, the set temperature range is 60-150 ℃.
Preferably, the treatment setting time is 2 hours or more;
preferably, the processing setting time is 4 hours or more.
4. The method according to any one of claims 1 to 3, wherein the medium comprises any one of water, high-pressure steam, an organic solvent, a potassium permanganate solution, an acid solution, an alkali solution, or a combination of at least two thereof;
preferably, the organic solvent comprises one or a mixed solvent of at least two of dimethylformamide, butanone, cyclohexanone, tetrahydrofuran, toluene, xylene or chloroform;
preferably, the acid solution comprises one or a mixed acid solution of at least two of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, acetic acid, formic acid, benzoic acid or permanganic acid;
preferably, the alkali liquor comprises one or a mixed alkali liquor of at least two of sodium hydroxide, potassium hydroxide, calcium hydroxide or ammonia water.
5. The method according to any one of claims 1 to 4, wherein the sample to be tested is placed in a medium for sample treatment by using a container with a medium reflux device;
preferably, when at least two samples are placed in the medium for processing, the samples are fixed in the container at intervals;
preferably, the interval fixing is performed by a clamping groove type device or a U-shaped groove device.
6. The method according to any one of claims 1 to 5, wherein the performing a test analysis on the sample-treated medium comprises qualitatively or quantitatively analyzing a sample-released substance in the sample-treated medium;
preferably, the medium after the sample is treated is tested and analyzed by any one or at least two of ion chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, gel chromatography, infrared spectroscopy and nuclear magnetic resonance analysis methods;
preferably, the test analysis of the treated medium is to compare the species and/or content of the released substances in at least two samples in parallel;
preferably, the step of performing the test analysis on the medium after the sample is processed comprises comparing the types and/or contents of the substances released by the samples in the processed medium of at least two different samples subjected to the same processing temperature and the same processing time, comparing the types and/or contents of the substances released by the samples in the processed medium of the same sample subjected to the same processing temperature and the same processing time, and comparing the types and/or contents of the substances released by the samples in the processed medium of the same sample subjected to the same processing temperature and the different processing times;
preferably, the step of performing test analysis on the medium after the sample is processed further includes setting a blank control, that is, performing the same treatment as the sample group to be tested on the medium without the sample to be tested, and analyzing the substance type and/or content in the medium after the blank treatment;
preferably, the test analysis of the treated medium comprises the treatment of a known benchmarking sample and a sample to be tested under the same treatment conditions, and the parallel comparison analysis of the type and/or content of released substances is carried out on the treated medium.
7. The method of any one of claims 1-6, further comprising performing a performance test analysis on the treated sample.
8. The method of any one of claim 7, wherein the performing a test analysis on the processed sample comprises analyzing any one or at least two of a change in a property of the sample before and after the processing, a rate of change in a weight of the sample before and after the processing, a change in a property of the processed sample compared to the same sample at different processing temperatures for the same processing time, or a change in a property of the processed sample compared to the same sample at the same processing temperature for the different processing time;
preferably, the step of performing test analysis on the processed sample comprises the steps of processing the target sample and the target sample under the same condition, and performing parallel comparison test and analysis on the performance change and the weight change rate of the target sample and the target sample;
preferably, the performance test on the sample comprises one or at least two of thermal stress limit, glass transition temperature, drop impact, interlayer adhesion, yellowness value, breakdown strength, dielectric constant and dielectric loss tangent, resistivity, signal delay, passive intermodulation PIM, flexural strength, flexural modulus, thermal decomposition temperature, coefficient of thermal expansion, thermal conductivity, dimensional stability, aging resistance, comparative tracking index, chemical migration resistance, or pressure resistance test.
9. Method according to any of claims 1-8, characterized in that the method comprises the steps of:
s1, pre-treating a sample to be tested, optionally etching copper foil, drilling and milling into a specific size and a specific pattern, washing with ultrapure water, drying in the air, and accurately weighing; s2, putting the pretreated sample into a container, adding a medium, heating to 40-300 ℃, and treating for more than 2 h; s3, taking out the processed sample from the container; s4, testing and analyzing the medium after the sample is processed, and analyzing the type and/or content of the released substances of the sample in the medium;
preferably, the method may further include S5, analyzing the change in the property of the sample before and after the treatment and the change rate of the weight of the sample before and after the treatment;
preferably, the vessel used in the method is provided with a medium return device;
preferably, the method provides for spacing the samples within the container when at least two samples are placed in the medium for processing.
10. Use of the method according to any one of claims 1-9 in reliability test analysis of a laminate or copper clad laminate, wherein the reliability analysis comprises a reliability analysis of heat resistance, ion migration resistance or pressure resistance.
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