CN110006778B - Method for detecting dispersibility of conductive paste for MLCC - Google Patents
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- CN110006778B CN110006778B CN201910356879.6A CN201910356879A CN110006778B CN 110006778 B CN110006778 B CN 110006778B CN 201910356879 A CN201910356879 A CN 201910356879A CN 110006778 B CN110006778 B CN 110006778B
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- G01N1/00—Sampling; Preparing specimens for investigation
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- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
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Abstract
The invention discloses a method for detecting the dispersibility of conductive paste for MLCC, which comprises the steps of coating the conductive paste to be detected on a smooth plastic film by using a film scraper to obtain a sample film with uniform surface and uniform thickness; putting the sample film and the plastic film into the center of an oven for drying; taking the dried sample film and the plastic film out of the oven; removing the plastic film on the dried sample film on clean paper, keeping the integrity of the dried sample film, and cutting the sample film into a plurality of sample films to be detected with equal length and width by a knife; and measuring each sample film to be measured by an MD-300S electronic specific gravity balance to obtain the dry film density corresponding to each sample to be measured, wherein the dry film density corresponding to the conductive paste to be detected is the average value of the measurement results. The method judges the dispersibility of the conductive paste according to the density of the dry film, can evaluate the dispersibility of the submicron conductive paste, and is quick and convenient.
Description
Technical Field
The invention relates to a method for detecting the dispersibility of conductive paste for MLCC, in particular to a method for detecting the dispersibility of conductive paste for submicron MLCC.
Background
The MLCC (Multi-layer Ceramic Capacitors), namely a chip type multilayer Ceramic capacitor, has the characteristics of outstanding advantages, small volume, compact structure, long service life, high reliability, suitability for Surface Mounting (SMT) and the like, so that the MLCC is more and more widely applied to the field. The development direction of the current chip multilayer ceramic capacitor (MLCC) is chip type, large capacity, low cost, miniaturization and high reliability, which puts higher requirements on the key raw materials of ceramic slurry and metal conductive slurry, because the ultrafine powder has larger specific surface area and higher surface energy, agglomeration and spontaneous agglomeration are easily generated, and how to evaluate the dispersibility after the ultrafine powder is made into the slurry is one of the difficulties.
The document CN104849410A discloses a method for rapidly detecting the dispersibility of titanium dioxide in an oil paint, which comprises the steps of sequentially adding an oil dispersant and the titanium dioxide into vegetable oil, uniformly stirring to obtain a mixed slurry, and detecting the dispersibility of the mixed slurry by using a scraper fineness meter. The formula for preparing the mixed slurry is simple, the cost is low, the added oily dispersing agents BYK-110 and BYK-161 have good dispersing effect on titanium dioxide, and the dispersing time can be effectively shortened. However, since the manufacturing error of the blade fineness gauge is in the micron order, it is difficult to judge the dispersion effect of the slurry in the submicron range by the method.
The document "a nickel paste and a method for producing the nickel paste" chinese patent No. CN 106575542B provides a nickel paste which has substantially no change in viscosity with time, is excellent in stability, and can be suitably used as an internal electrode of a laminated ceramic capacitor, and a method for producing the same. The content of the dispersion transfer accelerator having an anionic surfactant structure is 0.16 to 3.0 parts by mass per 100 parts by mass of the nickel powder, the content of the amine-based dispersion transfer accelerator is 0.2 to 4 times as high as that of the dispersion transfer accelerator having an anionic surfactant structure, the nickel concentration is 50 to 70% by mass, the viscosity is 8 to 150 pas, and the moisture percentage measured by the Karl Fischer method is less than 1% by mass. However, this patent only considers the viscosity and dispersion characteristics of the slurry itself, and does not evaluate the effect of dispersion.
The literature, "a method for detecting nickel powder dispersibility, chinese patent No. CN 103018264B" has the following operation steps: putting 3-5 g of nickel powder into a beaker, adding 170-190 ml of absolute ethyl alcohol, and carrying out ultrasonic treatment for 5-15 min while stirring in ultrasonic waves; standing and precipitating after the ultrasonic treatment is finished to enable layering to occur, wherein the upper layer is clear alcohol, and the lower layer is nickel powder slurry; taking out the nickel powder slurry on the lower layer to a glass slide, hanging the nickel powder slurry into a slurry belt with the length of 1-5 cm by using a slurry belt device, and drying the slurry belt together with the glass slide; putting the dried slurry belt and the slide into a sample chamber of a scanning electron microscope, adjusting parameters of the scanning electron microscope, and carrying out scanning shooting; and analyzing the pictures taken by scanning. The invention only detects the dispersibility of the raw materials, and the dispersibility of the prepared conductive paste cannot be evaluated.
Disclosure of Invention
The invention aims to provide a method for detecting the dispersibility of conductive paste for MLCC (multilayer ceramic capacitor) in the manufacturing and using process of the conductive paste. In view of the above object, the present inventors have made extensive studies to solve the above problems, and have found the following techniques to complete the present invention: for a powder, if the powder is better dispersed, the weight of the powder is larger under the same volume condition, if the powder is not well dispersed, the powder has a lot of soft agglomerates, and the piled powder has relatively light weight under the same volume condition.
The technical means adopted by the invention are as follows:
a method for detecting the dispersibility of conductive paste for MLCC comprises the following steps:
s1, coating the conductive paste to be detected on a smooth plastic film by using a film scraper to obtain a sample film with uniform surface and uniform thickness;
s2, putting the sample film and the plastic film into the center of an oven for drying to remove the solvent;
s3, taking the dried sample film and the plastic film out of the oven under the condition that the humidity outside the oven is less than 50%; if the humidity is too high, the sample film is liable to absorb moisture.
S4, removing the plastic film on the dried sample film on clean paper, keeping the integrity of the dried sample film, and cutting the sample film into a plurality of sample films to be detected with equal length and width by a knife;
and S5, measuring each sample film to be measured through an MD-300S electronic specific gravity balance to obtain the dry film density corresponding to each sample to be measured, wherein the dry film density corresponding to the conductive paste to be detected is the average value of the measurement results.
Before step S1, obtaining the thermal cracking temperature of each raw material component solvent of the conductive paste to be detected by a thermal difference analyzer, wherein the thermal cracking temperature with the highest temperature plus 1-5 ℃ is the drying temperature for drying in step S2, and the drying temperature is not too high for preventing oxidation.
The drying time in the step S2 is 2 hours, which ensures the sufficiency of volatilization.
The film scraper is of a cuboid structure, and the length, the width and the height of the film scraper are respectively 4cm, 4cm and 1 cm;
the film scraper is provided with square holes penetrating through the upper end face and the lower end face of the film scraper, and the length, the width and the height of each square hole are respectively 3cm, 3cm and 1 cm;
the bottom of the front end face of the film scraper is provided with a through groove communicated with the square hole, the left groove wall of the through groove and the left hole wall of the square hole are positioned on the same plane, the right groove wall of the through groove and the right hole wall of the square hole are positioned on the same plane, and the groove depth of the through groove is 20 micrometers;
in step S1, the step of applying the conductive paste to be detected on the smooth plastic film by the film scraper is as follows: the film scraper is arranged on the plastic film, the square hole is filled with the conductive slurry to be detected, the front end face of the film scraper is arranged at the back, the rear end face of the film scraper is arranged at the front, the film scraper is dragged along a straight line to coat the conductive slurry to be detected on the smooth plastic film, the middle part of the conductive slurry to be detected coated on the smooth plastic film is cut, and the sample film with uniform surface and uniform thickness is obtained. The arrangement of the film scraper ensures the consistency of the width and the thickness of the thin film of the sample.
The plastic film is a PET film.
The method judges the dispersibility of the conductive paste according to the density of the dry film, can evaluate the dispersibility of the submicron conductive paste, and is quick and convenient.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is an optical micrograph of a sample 1 according to an embodiment of the present invention.
FIG. 2 is an optical micrograph of sample 2 according to the embodiment of the present invention.
FIG. 3 is an optical micrograph of sample 3 according to the embodiment of the present invention.
FIG. 4 is a top view of a wiper according to an embodiment of the present invention.
FIG. 5 is a side view of a film scraper in an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for detecting the dispersibility of conductive paste for MLCC comprises the following steps:
s1, obtaining a thermal cracking temperature of a solvent of each raw material component (dispersant, organic solvent, plasticizer, metal powder, inorganic additive, etc.) of the conductive paste to be detected by using a thermal difference analyzer, wherein the thermal cracking temperature with the highest temperature plus 1-5 ℃ is a drying temperature for drying, and in this embodiment, the drying temperature is 200 ℃.
S2, coating the conductive paste to be detected on a smooth PET film by using a film scraper to obtain a sample film with a uniform surface and a uniform thickness, wherein the film scraper is of a cuboid structure and has a length, a width and a height of 4cm, 4cm and 1cm respectively as shown in figures 4 and 5; the film scraper is provided with a square hole 1 penetrating through the upper end surface and the lower end surface of the film scraper, and the length, the width and the height of the square hole 1 are respectively 3cm, 3cm and 1 cm; the bottom of the front end face of the film scraper is provided with a through groove 2 communicated with the square hole 1, the left groove wall of the through groove 2 and the left hole wall of the square hole 1 are positioned on the same plane, the right groove wall of the through groove 2 and the right hole wall of the square hole 1 are positioned on the same plane, and the groove depth of the through groove 2 is 20 micrometers;
the method comprises the following specific steps of coating the conductive paste to be detected on a smooth PET film by using a film scraper: the film scraper is arranged on a PET (polyethylene terephthalate) film, the square hole 1 is filled with conductive paste to be detected, the front end face of the film scraper is back, the rear end face of the film scraper is front, the film scraper is dragged along a straight line to coat the conductive paste to be detected on the smooth PET film, the middle part of the conductive paste to be detected coated on the smooth PET film is cut, and a sample film with a uniform surface and a uniform thickness is obtained, wherein the thickness of the sample film is 20 micrometers, the length of the sample film is 30cm, and the width of the sample film is 3 cm;
s3, putting the sample film and the PET film into the center of an oven for drying at the temperature of 200 ℃ for 2 hours to remove the solvent;
s3, taking out the dried sample film and the PET film from the oven by using tweezers under the condition that the humidity outside the oven is less than 50%;
s4, removing the PET film on the dried sample film on clean paper, keeping the integrity of the dried sample film, and cutting the sample film into ten sample films to be detected with the length and width of 3cm multiplied by 3cm by a knife;
and S5, measuring each sample film to be measured through an MD-300S electronic specific gravity balance to obtain the dry film density corresponding to each sample to be measured, wherein the dry film density corresponding to the conductive paste to be detected is the average value of the measurement results.
The conductive paste to be detected is as follows:
the conductive pastes of samples 1-3 have the same particle size and different stirring conditions, and are stirred insufficiently, normally and very sufficiently. The morphology of samples 1-3 was observed as shown in FIGS. 1-3: sample 1 (under stirring) had significant agglomeration, while sample 2 (under stirring) had significantly less agglomeration, but it was difficult to confirm whether dispersion achieved the effect; sample 3 (stirred very well) had no visible agglomeration, but the quality of the dispersion was not measured by a quantitative indicator.
The dry film densities for samples 1-12 obtained by the above method were as follows:
the dispersibility of the conductive paste can be judged according to the dry film density (Mean) corresponding to each sample, the method is rapid and convenient, and the dispersibility of the conductive paste in submicron order can be evaluated.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. A method for detecting the dispersibility of conductive paste for MLCC is characterized by comprising the following steps:
s1, coating the conductive paste to be detected on a smooth plastic film by using a film scraper to obtain a sample film with uniform surface and uniform thickness;
s2, putting the sample film and the plastic film into the center of an oven for drying to remove the solvent;
s3, taking the dried sample film and the plastic film out of the oven under the condition that the humidity outside the oven is less than 50%;
s4, removing the plastic film on the dried sample film on clean paper, keeping the integrity of the dried sample film, and cutting the sample film into a plurality of sample films to be detected with equal length and width by a knife;
s5, measuring each sample film to be measured through an MD-300S electronic specific gravity balance to obtain the dry film density corresponding to each sample to be measured, wherein the dry film density corresponding to the conductive paste to be detected is the average value of the measurement results; the conductive paste is changed from a liquid state to a powder state, the dry film density is obtained under the condition that the powder characteristics of the original paste are not damaged, if the density is higher, the dispersibility of the conductive paste is indirectly shown to be better, and then the dispersibility of the conductive paste in the submicron level can be evaluated.
2. The method of detecting dispersibility of conductive paste for MLCCs according to claim 1, wherein: before step S1, obtaining thermal cracking temperatures of the solvents of the raw material components of the conductive paste to be detected by using a thermal difference analyzer, wherein the thermal cracking temperature with the highest temperature plus 1-5 ℃ is the drying temperature in step S2.
3. The method of detecting dispersibility of conductive paste for MLCCs according to claim 2, wherein: the drying time of the drying in the step S2 is 2 hours.
4. The method of detecting dispersibility of conductive paste for MLCCs according to claim 1, wherein: the film scraper is of a cuboid structure, and the length, the width and the height of the film scraper are respectively 4cm, 4cm and 1 cm;
the film scraper is provided with square holes penetrating through the upper end face and the lower end face of the film scraper, and the length, the width and the height of each square hole are respectively 3cm, 3cm and 1 cm;
the bottom of the front end face of the film scraper is provided with a through groove communicated with the square hole, the left groove wall of the through groove and the left hole wall of the square hole are positioned on the same plane, the right groove wall of the through groove and the right hole wall of the square hole are positioned on the same plane, and the groove depth of the through groove is 20 micrometers;
in step S1, the step of applying the conductive paste to be detected on the smooth plastic film by the film scraper is as follows: the film scraper is arranged on the plastic film, the square hole is filled with the conductive slurry to be detected, the front end face of the film scraper is arranged at the back, the rear end face of the film scraper is arranged at the front, the film scraper is dragged along a straight line to coat the conductive slurry to be detected on the smooth plastic film, the middle part of the conductive slurry to be detected coated on the smooth plastic film is cut, and the sample film with uniform surface and uniform thickness is obtained.
5. The method of detecting dispersibility of conductive paste for MLCCs according to claim 1, wherein: the plastic film is a PET film.
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| CN110806364A (en) * | 2019-11-05 | 2020-02-18 | 江苏博迁新材料股份有限公司 | Method for detecting density of copper sheet drying film |
| CN110907310A (en) * | 2019-12-11 | 2020-03-24 | 广州立邦涂料有限公司 | Method for detecting density of automobile coating dry film |
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