CN110006778A - A method of detection MLCC electrocondution slurry dispersibility - Google Patents
A method of detection MLCC electrocondution slurry dispersibility Download PDFInfo
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- CN110006778A CN110006778A CN201910356879.6A CN201910356879A CN110006778A CN 110006778 A CN110006778 A CN 110006778A CN 201910356879 A CN201910356879 A CN 201910356879A CN 110006778 A CN110006778 A CN 110006778A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/36—Analysing materials by measuring the density or specific gravity, e.g. determining quantity of moisture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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Abstract
The invention discloses a kind of methods for detecting MLCC electrocondution slurry dispersibility, and electrocondution slurry to be detected is applied on smooth plastic film with blade applicator, obtain that surface is uniform and sample thin film in homogeneous thickness；Sample thin film is put into baking oven center together with plastic film together to dry；The sample thin film dried is taken out from baking oven together with plastic film；On clean paper, the plastic film on the sample thin film dried is taken off, keep the sample thin film integrality dried, be cut into multiple sample to be tested films that length and width is equal with the above-mentioned sample thin film of hilt；Each sample to be tested film is measured by MD-300S electronics specific gravity balance, obtains the corresponding dry- film density of each sample to be tested, and dry- film density corresponding to electrocondution slurry to be detected is the average value of above-mentioned measurement result.The present invention judges electrocondution slurry dispersibility quality by dry- film density size, and can assess the dispersibility of the electrocondution slurry of submicron order, and method is quick, convenient.
Description
Technical field
The present invention relates to a kind of methods for detecting MLCC electrocondution slurry dispersibility, specifically detection submicron order
The method of MLCC electrocondution slurry dispersibility.
Background technique
MLCC (Multi-layer Ceramic Capacitors) i.e. chip multilayer ceramic capacitor, MLCC product advantage
It is prominent, it is small in size, compact-sized, the service life is long, high reliablity and the features such as being suitable for surface installation (SMT) make it in application field
It is increasingly wider.The developing direction of current chip multilayer ceramic capacitor (MLCC) is chip type, large capacity, low cost, miniaturization
And high reliability, this puts forward higher requirements its key raw material ceramic slurry and metal conductive paste, due to superfine powder
Body have biggish specific surface area and higher surface can, easily generate and reunite and spontaneous cohesion, be made into after slurry how to point
It is one of its difficult point that scattered property, which carries out evaluation,.
Document " a kind of titanium dioxide dispersed rapid detection method CN104849410A " in oil paint discloses one
Dispersed rapid detection method of the kind titanium dioxide in oil paint, is added sequentially to vegetable oil for oiliness dispersing agent and titanium dioxide
In, mixed slurry is obtained after mixing evenly, with the dispersibility of Hegman grind gage detection mixed slurry.This method prepares mixed slurry
Formula it is simple, cost is relatively low, wherein oiliness dispersant B YK-110, the BYK-161 being added to titanium dioxide have well dispersion effect
Fruit, can effectively shorten jitter time.But just in the micron-scale due to Hegman grind gage foozle itself, this method is to sub-micron
Slurry be difficult to judge the effect of its dispersion.
Document " Chinese patent that the manufacturing method grant number of nickel cream and nickel cream is CN 106575542B " provides a kind of viscosity
It is basic without ongoing change, excellent in stability, can suitably serve as laminated ceramic capacitor internal electrode nickel cream and
Its manufacturing method.The content of split-up promotor with the anionic interfacial agent structure is relative to nickel powder 100
Mass parts are 0.16 mass parts~3.0 mass parts, and the content of amine system split-up promotor is with anionic interfacial activity
0.2 times of the split-up promotor of agent structure~4 times, in addition, nickel concentration is the 50 mass % of mass %~70, viscosity is
8Pas~150Pas, the moisture rate measured by Karl_Fischer method is less than 1 mass %.But this patent only considers slurry
The viscosity and dispersing characteristic of itself, do not evaluate the effect that it disperses.
Document " Chinese patent that a kind of method grant number for detecting dispersity of nickel powder is CN 103018264B " has following
Operating procedure: taking 3~5g nickel powder into beaker, be added 170~190ml dehydrated alcohol, in ultrasonic wave while stirring ultrasound 5~
15min；It is staticly settled after the completion of ultrasound, makes to be layered, be at the middle and upper levels clarifying potable, lower layer is nickel powder slurry；It takes
Out on the nickel powder slurry to slide of lower layer, nickel powder slurry is hung to the slurry band that 1~5cm long is made with slurrying material strip equipment, then
Slurry band is dried together with slide；Slurry band after drying is put into the sample room of scanning electron microscope together with slide
It is interior, scanning electron microscope parameter is adjusted, shooting is scanned；The photo of scanning shoot is analyzed.The invention is only examined
The dispersibility for having surveyed raw material not can be carried out assessment to the dispersibility that electrocondution slurry is made.
Summary of the invention
It is an object of the invention to provide a kind of detection MLCC electrocondution slurry point in electrocondution slurry manufacture use process
Dissipate the method for property.Based on above-mentioned purpose, the discussion for solving the above problems has been repeated, has found following technologies to complete
The present invention: for a powder, if its dispersion is better, weight will be bigger under the conditions of same volume, such as
Fruit dispersion it is bad, powder has many soft-agglomerated, and the powder that heap comes will weight relatively light one under the conditions of same volume
A bit, we can use this principle in the dispersion of electrocondution slurry, and an electrocondution slurry of trying every possible means becomes powdered form from liquid,
Guarantee obtains dry- film density under conditions of not destroying its powder characteristics of original slurry, if the density the big can so to show indirectly
Electrocondution slurry dispersibility is better, and then can assess the dispersibility of the electrocondution slurry of submicron order.
The technological means that the present invention uses is as follows:
A method of detection MLCC electrocondution slurry dispersibility has following steps:
S1, electrocondution slurry to be detected is applied on smooth plastic film with blade applicator, obtains surface uniformly and thickness
Uniform sample thin film；
S2, it sample thin film is put into baking oven center together with plastic film together dries, to remove solvent；
S3, under conditions of humidity is less than 50% outside baking oven, by the sample thin film dried together with plastic film from baking oven
Middle taking-up；If humidity is excessive, sample thin film easily absorbs moisture.
S4, on clean paper, take the plastic film on sample thin film dry, the sample thin film that holding has been dried off
Integrality is cut into multiple sample to be tested films that length and width is equal with the above-mentioned sample thin film of hilt；
S5, each sample to be tested film are measured by MD-300S electronics specific gravity balance, obtain each sample to be tested pair
The dry- film density answered, dry- film density corresponding to electrocondution slurry to be detected are the average value of above-mentioned measurement result.
Before step S1, the thermal cracking of each raw material component solvent of electrocondution slurry to be detected is obtained by heating differential analysis instrument
Temperature, wherein the highest thermal cracking temperature of temperature adds 1-5 DEG C to be the drying temperature dried in the step S2, for anti-block
Change, drying temperature is unsuitable excessively high.
The drying time dried in the step S2 is 2 hours, ensure that the adequacy of volatilization.
The blade applicator is in rectangular parallelepiped structure, and length, width and height are respectively 4cm, 4cm and 1cm；
The blade applicator has the square hole for penetrating through end face and lower end surface thereon, and the length, width and height of the square hole are respectively 3cm,
3cm and 1cm；
Blade applicator front end face bottom has the through slot being connected to the square hole, the left cell wall of the through slot and the side
The left hole wall in hole is generally aligned in the same plane, and the right cell wall of the through slot is generally aligned in the same plane with the right hole wall of the square hole, and described
The groove depth of through slot is 20 μm；
In the step S1, the specific steps that are applied to electrocondution slurry to be detected with blade applicator on smooth plastic film
As follows: the blade applicator is placed on plastic film, fills the square hole with electrocondution slurry to be detected, the blade applicator front end face exists
Afterwards, the blade applicator rear end face drags the blade applicator along straight line and electrocondution slurry to be detected is applied to smooth plastics preceding
On film, the middle section for the electrocondution slurry to be detected being applied on smooth plastic film is intercepted, it is uniformly and thick to obtain surface
Spend uniform sample thin film.The setting of the blade applicator ensure that the consistency of sample thin film width and thickness.
The plastic film is PET film.
The present invention judges electrocondution slurry dispersibility quality by dry- film density size, and can be to the conductive paste of submicron order
The dispersibility of material is assessed, and method is quick, convenient.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to do simply to introduce, it should be apparent that, the accompanying drawings in the following description is this hair
Bright some embodiments for those of ordinary skill in the art without any creative labor, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the optical microscope photograph of sample 1 in a specific embodiment of the invention.
Fig. 2 is the optical microscope photograph of sample 2 in a specific embodiment of the invention.
Fig. 3 is the optical microscope photograph of sample 3 in a specific embodiment of the invention.
Fig. 4 is the top view of blade applicator in a specific embodiment of the invention.
Fig. 5 is the side view of blade applicator in a specific embodiment of the invention.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
A method of detection MLCC electrocondution slurry dispersibility has following steps:
S1, each raw material component (dispersing agent, organic solvent, the plasticizing that electrocondution slurry to be detected is obtained by heating differential analysis instrument
Agent, metal powder and inorganic additive etc.) solvent thermal cracking temperature, wherein the highest thermal cracking temperature of temperature add 1-5 DEG C be
The drying temperature of drying, in the present embodiment, drying temperature is 200 DEG C.
S2, electrocondution slurry to be detected is applied on smooth PET film with blade applicator, obtains that surface is uniform and thickness is uniform
Sample thin film, as shown in Figure 4 and Figure 5, the blade applicator be in rectangular parallelepiped structure, length, width and height are respectively 4cm, 4cm and 1cm；
The blade applicator has a square hole 1 of perforation end face and lower end surface thereon, and the length, width and height of the square hole 1 are respectively 3cm, 3cm and
1cm；Blade applicator front end face bottom has the through slot 2 being connected to the square hole 1, the left cell wall of the through slot 2 and the side
The left hole wall in hole 1 is generally aligned in the same plane, and the right cell wall of the through slot 2 and the right hole wall of the square hole 1 are generally aligned in the same plane, and institute
The groove depth for stating through slot 2 is 20 μm；
Electrocondution slurry to be detected is applied on smooth PET film to specific step is as follows: the blade applicator with blade applicator
It is placed on PET film, fills the square hole 1 with electrocondution slurry to be detected, the blade applicator front end face is in rear, the blade applicator rear end
Face drags the blade applicator along straight line and electrocondution slurry to be detected is applied on smooth PET film preceding, and interception is applied to smooth
PET film on electrocondution slurry to be detected middle section, obtain that surface is uniform and sample thin film in homogeneous thickness, the sample
Film thickness is 20 μm, length 30cm, width 3cm；
S3, it sample thin film is put into baking oven center together with PET film together dries, drying temperature is 200 DEG C, when drying
Between be 2 hours, to remove solvent；
S3, under conditions of humidity is less than 50% outside baking oven, with tweezers by the sample thin film dried together with PET film from baking
It is taken out in case；
S4, on clean paper, take the PET film on sample thin film dry off, the sample thin film that holding has been dried is complete
Whole property is cut into ten sample to be tested films that length and width is 3cm × 3cm with the above-mentioned sample thin film of hilt；
S5, each sample to be tested film are measured by MD-300S electronics specific gravity balance, obtain each sample to be tested pair
The dry- film density answered, dry- film density corresponding to electrocondution slurry to be detected are the average value of above-mentioned measurement result.
Electrocondution slurry to be detected is as follows:
The electrocondution slurry partial size of sample 1-3 is identical, and stirring state is different, respectively stirs insufficient, and stirring generally and is stirred
It mixes very sufficiently.The pattern of sample 1-3 is observed, as shown in Figs. 1-3: sample 1 (stirring is insufficient) has apparent reunion, sample 2
(stirring is general), which reunites, obviously to become smaller, but it is difficult to confirm whether dispersion reaches effect；Sample 3 (stirring is very abundant) has been seen not
To reunion, but the index of quality none quantization dispersed is measured.
It is as follows that dry- film density corresponding to sample 1-12 is obtained by the above method:
It can determine whether that electrocondution slurry dispersibility quality, method are fast by dry- film density corresponding to each sample (Mean) size
It is fast, convenient, and the dispersibility of the electrocondution slurry of submicron order can be assessed.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (5)
1. a kind of method for detecting MLCC electrocondution slurry dispersibility, it is characterised in that have following steps:
S1, electrocondution slurry to be detected is applied on smooth plastic film with blade applicator, obtains that surface is uniform and thickness is uniform
Sample thin film；
S2, it sample thin film is put into baking oven center together with plastic film together dries, to remove solvent；
S3, under conditions of humidity is less than 50% outside baking oven, the sample thin film dried is taken from baking oven together with plastic film
Out；
S4, on clean paper, take the plastic film on sample thin film dry off, the sample thin film that holding has been dried is complete
Property, multiple sample to be tested films that length and width is equal are cut into the above-mentioned sample thin film of hilt；
S5, each sample to be tested film are measured by MD-300S electronics specific gravity balance, and it is corresponding to obtain each sample to be tested
Dry- film density, dry- film density corresponding to electrocondution slurry to be detected are the average value of above-mentioned measurement result.
2. it is according to claim 1 detection MLCC electrocondution slurry dispersibility method, it is characterised in that: step S1 it
Before, the thermal cracking temperature of each raw material component solvent of electrocondution slurry to be detected is obtained by heating differential analysis instrument, wherein temperature highest
Thermal cracking temperature add 1-5 DEG C to be the drying temperature dried in the step S2.
3. the method for detection MLCC electrocondution slurry dispersibility according to claim 2, it is characterised in that: the step S2
The drying time of middle drying is 2 hours.
4. the method for detection MLCC electrocondution slurry dispersibility according to claim 1, it is characterised in that: the blade applicator
In rectangular parallelepiped structure, length, width and height are respectively 4cm, 4cm and 1cm；
The blade applicator has a square hole of perforation end face and lower end surface thereon, and the length, width and height of the square hole are respectively 3cm, 3cm and
1cm；
Blade applicator front end face bottom has the through slot being connected to the square hole, left cell wall and the square hole of the through slot
Left hole wall is generally aligned in the same plane, and the right cell wall of the through slot is generally aligned in the same plane with the right hole wall of the square hole, and the through slot
Groove depth be 20 μm；
In the step S1, electrocondution slurry to be detected is applied to specific steps on smooth plastic film with blade applicator such as
Under: the blade applicator is placed on plastic film, fills the square hole with electrocondution slurry to be detected, the blade applicator front end face exists
Afterwards, the blade applicator rear end face drags the blade applicator along straight line and electrocondution slurry to be detected is applied to smooth plastics preceding
On film, the middle section for the electrocondution slurry to be detected being applied on smooth plastic film is intercepted, it is uniformly and thick to obtain surface
Spend uniform sample thin film.
5. the method for detection MLCC electrocondution slurry dispersibility according to claim 1, it is characterised in that: the plastics are thin
Film is PET film.
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| CN201910356879.6A CN110006778B (en) | 2019-04-29 | 2019-04-29 | Method for detecting dispersibility of conductive paste for MLCC |
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| CN201910356879.6A CN110006778B (en) | 2019-04-29 | 2019-04-29 | Method for detecting dispersibility of conductive paste for MLCC |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN110006778B (en) | 2021-11-26 |
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