CN104174841B - Superelevation holds manufacture method and nickel slurry, the MLCC that MLCC starches with nickel - Google Patents
Superelevation holds manufacture method and nickel slurry, the MLCC that MLCC starches with nickel Download PDFInfo
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- CN104174841B CN104174841B CN201410407267.2A CN201410407267A CN104174841B CN 104174841 B CN104174841 B CN 104174841B CN 201410407267 A CN201410407267 A CN 201410407267A CN 104174841 B CN104174841 B CN 104174841B
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- superelevation
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Abstract
The invention discloses a kind of superelevation and hold the manufacture method of MLCC nickel slurry, comprise the following steps: (1) takes nikel powder, dispersant and solvent, disperses with sand mill；(2) take barium titanate powder, dispersant and solvent, disperse with sand mill；(3) by step (1), the mixing of (2) gained material, add binding agent and be stirred；(4) conventional disperse, filtration.Present invention also offers the nickel slurry that a kind of manufacture method using superelevation to hold MLCC nickel slurry obtains, and a kind of MLCC prepared by superelevation appearance MLCC nickel slurry.The method of the present invention improves the powder body dispersion effect of nikel powder and barium titanate powder, and prepared MLCC product is pressure, HALT is functional.
Description
Technical field
The present invention relates to superelevation and hold the manufacture method of MLCC nickel slurry, hold MLCC nickel particularly to superelevation
The process for dispersing of slurry.The invention still further relates to be held, by superelevation, the nickel slurry that the preparation method of MLCC nickel slurry obtains,
And the MLCC prepared is starched by this nickel.
Background technology
At present, superelevation hold multiple-layer sheet ceramic capacitor (MLCC) product such as 0402X5R225,
The nickel slurry that 0805X5R226 etc. use, it is desirable to nikel powder particle diameter is 0.17～0.20 μm, and barium titanate powder particle diameter is
0.05～0.1 μm.The particle diameter that powder body is the least becomes the highest to dispersion requirement.If dispersion effect is bad, then
Nickel slurry exists the bulky grain of reunion and can cause that product is pressure, Highly Accelerated Life Test (HALT) penalty,
Even result in and scrap.
The general technology flow process that at present nickel slurry makes is: by nikel powder, barium titanate powder and dispersant, binding agent,
After solvent is mixed together stirring, then roll slurry dispersion with three-high mill.The high nickel slurry that holds so made often reaches not
To the dispersion effect needed so that product is pressure, HALT poor performance.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of superelevation and hold the making side of MLCC nickel slurry
Method, be the technical scheme is that
Superelevation holds the manufacture method that MLCC starches with nickel, comprises the following steps:
(1) take nikel powder, dispersant and solvent, disperse with sand mill；
(2) take barium titanate powder, dispersant and solvent, disperse with sand mill；
(3) by step (1), the mixing of (2) gained material, add binding agent and be stirred；
(4) conventional disperse, filtration.
Preferably, it is dispersed under 1500-2500rpm described in step (1), (2) and carries out, it is highly preferred that point
Dissipate 2 ± 0.5h.
Preferably, in step (1), the addition of nikel powder is the 40-70% of step (1) material gross weight,
The addition of dispersant is the 0.3-2% of gross weight, and surplus is solvent.
Preferably, in step (2), the addition of barium titanate powder is the 40-70% of step (2) material gross weight,
The addition of dispersant is the 0.3-2% of gross weight, and surplus is solvent.
Preferably, dispersant described in step (1), (2) is phosphoric acid ester dispersant, Span series, gathers
One or more in carboxylic acid series, lecithin etc..
Preferably, solvent described in step (1), (2) is dodecane, dibutyl phthalate, adjacent benzene
One in dioctyl phthalate dioctyl ester, capryl alcohol, terpineol, benzyl alcohol, diethylene glycol monobutyl ether, menthol or
Multiple.
Preferably, step (3) described binding agent be concentration be the ethyl cellulose solution of 8～20%.Preferably,
By ethyl cellulose resin solvent dodecane, dibutyl phthalate, dioctyl phthalate, pungent
One or more in alcohol, terpineol, benzyl alcohol, diethylene glycol monobutyl ether, menthol are dissolved, and make ethyl
Cellulose concentration (w/v) is 8-20%, prepares binding agent.
Preferably, step (1) and (2) use identical solvent.Preferably, in step (3), preparation is viscous
The solvent phase that the solvent of mixture and step (1) and/or (2) use is same.It is highly preferred that step (1) and (2)
The solvent of preparation binding agent in identical solvent, and step (3) is used also to make with step (1) and (2)
Solvent phase with.
Preferably, step (1) material gross weight, step (2) material gross weight and step (3) are described viscous
The ratio of mixture weight is 100:(10-30): (20-40).
Preferably, step (4) described conventional disperse is ground dispersion for employing three-high mill, it is highly preferred that
Dispersion 5 ± 0.5h.
Preferably, secondary filter is carried out by filter element after being filtered into dilution described in step (4).
Present invention also offers the nickel slurry that a kind of manufacture method using superelevation to hold MLCC nickel slurry obtains.
It addition, present invention also offers a kind of MLCC prepared by superelevation appearance MLCC nickel slurry.Preparation side
The method that method prepares MLCC with common nickel slurry is identical.
The invention has the beneficial effects as follows:
Nikel powder is stirred together with barium titanate powder, disperses through milling train by the nickel slurry dispersing technology of prior art, but real
On border, nikel powder and barium titanate powder particle diameter are different, and dispersion requires the most different, cannot when both being disperseed together
Ensure that two kinds of powder body are all completely dispersed simultaneously.After nikel powder and barium titanate powder are disperseed by the present invention respectively with sand mill
Remix stirring, roll slurry together, effectively improve the dispersion effect of powder body.Prepared by manufacture method of the present invention
Nickel slurry good dispersion, it is possible to meet preparation superelevation hold MLCC requirement.Nickel of the present invention slurry is utilized to prepare
MLCC product excellent electrical property, the most pressure functional, HALT performance is relative to prior art products
Have and be obviously improved.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of the front nikel powder of dispersion；
Fig. 2 is the SEM figure of nickel slurry after embodiment 1 is disperseed；
Fig. 3 is the SEM figure of nickel slurry after embodiment 2 is disperseed；
Fig. 4 is the SEM figure of nickel slurry after embodiment 3 is disperseed.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.Following example are only for example, not
Limitation of the present invention.That makes on the basis of the present invention replaces on an equal basis, modifies or changes, and each falls within this
In bright protection domain.
Embodiment 1
Make superelevation appearance MLCC nickel by the following method to starch:
(1) nikel powder of 40 parts is taken by weight, the phosphoric acid ester dispersant Hostaphat OPS 75E of 0.3 part
And the dodecane of 59.7 parts, it is placed in sand mill, disperses 2 hours in 1500rpm.
(2) barium titanate powder of 40 parts is taken by weight, the phosphoric acid ester dispersant Hostaphat OPS 75E of 0.3 part
And the dodecane of 59.7 parts；Herein, the gross weight of barium titanate powder, dispersant and dodecane is step (1)
The 10% of material gross weight.Material is placed in sand mill, disperses 2 hours in 1500rpm.
(3) material of step (1) and (2) is mixed, and add binding agent and be stirred；Wherein bond
The preparation method of agent is: is dissolved by ethyl cellulose resin dodecane, makes the concentration (w/v) of ethyl cellulose
It is 8%.The addition of binding agent is the 20% of step (1) material gross weight.
(4) three-high mill grinding distribution is used 5 hours.
(5) carry out secondary filter by filter element after dilution, thoroughly remove bulky grain.
Embodiment 2
Make superelevation appearance MLCC nickel by the following method to starch:
(1) take by weight the nikel powder of 55 parts, the phosphoric acid ester dispersant Hostaphat OPS 75E of 0.5 part,
0.5 part of Span series dispersant S-40, the capryl alcohol of 22 parts, terpineol of 22 parts, be placed in sand mill, in
2000rpm disperses 2.5 hours.
(2) barium titanate powder of 51 parts is taken by weight, the phosphoric acid ester dispersant Hostaphat OPS of 0.5 part
75E, 0.5 part of Span series dispersant S-40, the capryl alcohol of 24 parts, terpineol of 24 parts；Material herein is total
Weight is the 20% of step (1) material gross weight.Material is placed in sand mill, disperses in 2000rpm
2.5 hour.
(3) material of step (1) and (2) is mixed, and add binding agent and be stirred；Wherein bond
The preparation method of agent is: is dissolved by ethyl cellulose resin capryl alcohol, makes the concentration (w/v) of ethyl cellulose
It is 15%.The addition of binding agent is the 30% of step (1) material gross weight.
(4) three-high mill grinding distribution is used 5.5 hours.
(5) carry out secondary filter by filter element after dilution, thoroughly remove bulky grain.
Embodiment 3
Make superelevation appearance MLCC nickel by the following method to starch:
(1) take the nikel powder of 70 parts, 2 parts of lecithin, 28 parts of menthols by weight, be placed in sand mill,
Disperse 1.5 hours in 2500rpm.
(2) barium titanate powder of 70 parts, 2 parts of lecithin, 28 parts of menthols are taken by weight；Barium titanate powder,
The gross weight of lecithin and menthol is the 30% of step (1) material gross weight.Material is placed in sand mill,
Disperse 1.5 hours in 2500rpm.
(3) material of step (1) and (2) is mixed, and add binding agent and be stirred；Wherein bond
The preparation method of agent is: is dissolved by ethyl cellulose resin menthol, makes the concentration (w/v) of ethyl cellulose
It is 20%.The addition of binding agent is the 40% of step (1) material gross weight.
(4) three-high mill grinding distribution is used 4.5 hours.
(5) carry out secondary filter by filter element after dilution, thoroughly remove bulky grain.
Embodiment 4
Take the nikel powder before dispersion and the nickel slurry after the dispersion of embodiment 1-3, see under a scanning electron microscope
Examine.Result is as shown in Figure 1, Figure 2, Figure 3 and Figure 4.Fig. 1 is the SEM figure of the nikel powder before dispersion, figure
2-4 is the SEM figure of the nickel slurry after embodiment 1,2,3 dispersion respectively.By the SEM figure of Fig. 2-4 and Fig. 1
Contrasting visible, in embodiment of the present invention 1-3, nikel powder and barium titanate powder are completely dispersed, and nickel slurry dispersion effect is good.
Embodiment 5
The nickel slurry that nickel prepared by Example 1-3 is starched and prepared by prior art, respectively makes
80 (0402X5R105) MLCC products, test the electrical property of all products under the same conditions.Wherein,
Nickel slurry prepared by prior art refers to be mixed together nikel powder, barium titanate powder and dispersant, binding agent, solvent
After stirring, then roll the nickel slurry starching dispersion and obtain with three-high mill.Test result is as shown in table 1:
Table 1 embodiment 1-3 and prior art nickel slurry prepare the electrical property of MLCC product
Wherein, Cp is capacitance, and Df is dissipation factor, and BDV is breakdown voltage, and IR is insulation impedance value,
Halt is Highly Accelerated Life Test.From table 1, relative to the MLCC of prior art nickel slurry preparation, this
The Cp of the MLCC of the nickel slurry preparation of inventive embodiments 1-3 is relatively big, BDV is higher, and HALT performance has aobvious
Write and promote, the excellent electrical property of product.
Claims (8)
1. superelevation holds the manufacture method that MLCC starches with nickel, comprises the following steps:
(1) take nikel powder, dispersant and solvent, disperse with sand mill；The addition of nikel powder is step (1)
The 40-70% of material gross weight, the addition of dispersant is the 0.3-2% of gross weight, and surplus is solvent；
(2) take barium titanate powder, dispersant and solvent, disperse with sand mill；The addition of barium titanate powder
For the 40-70% of step (2) material gross weight, the addition of dispersant is the 0.3-2% of gross weight, remaining
Amount is solvent；
(3) by step (1), the mixing of (2) gained material, add binding agent and be stirred；
(4) conventional disperse, filtration.
Superelevation the most according to claim 1 holds the manufacture method of MLCC nickel slurry, it is characterised in that: step
(1), (2) described dispersion is dispersion 2 ± 0.5h under 1500-2500rpm.
Superelevation the most according to claim 1 holds the manufacture method of MLCC nickel slurry, it is characterised in that: step
(1), dispersant described in (2) is phosphoric acid ester dispersant, Span series, polycarboxylic acids series, ovum phosphorus
One or more in fat.
Superelevation the most according to claim 1 holds the manufacture method of MLCC nickel slurry, it is characterised in that: step
(1), solvent described in (2) be dodecane, dibutyl phthalate, dioctyl phthalate,
One or more in capryl alcohol, terpineol, benzyl alcohol, diethylene glycol monobutyl ether, menthol.
Superelevation the most according to claim 1 holds the manufacture method of MLCC nickel slurry, it is characterised in that: step
(3) described binding agent be concentration be the ethyl cellulose solution of 8～20%.
Superelevation the most according to claim 1 holds the manufacture method of MLCC nickel slurry, it is characterised in that: step
(1) ratio of material gross weight, step (2) material gross weight and step (3) binder wt is 100:
(10-30): (20-40).
7. a superelevation is held MLCC nickel and is starched, it is characterised in that described nickel slurry is by any one of claim 1～6 institute
The manufacture method stated is prepared.
8. a MLCC, it is characterised in that described MLCC is starched by the nickel described in claim 7 and is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410407267.2A CN104174841B (en) | 2014-08-18 | 2014-08-18 | Superelevation holds manufacture method and nickel slurry, the MLCC that MLCC starches with nickel |
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|---|---|---|---|
| CN201410407267.2A CN104174841B (en) | 2014-08-18 | 2014-08-18 | Superelevation holds manufacture method and nickel slurry, the MLCC that MLCC starches with nickel |
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| CN104174841A CN104174841A (en) | 2014-12-03 |
| CN104174841B true CN104174841B (en) | 2016-08-24 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109830373A (en) * | 2019-03-27 | 2019-05-31 | 大连海外华昇电子科技有限公司 | A kind of multilayer ceramic capacitor slurry fast matching method for downstream producer slurry shrinking percentage |
| CN116313512B (en) * | 2023-05-19 | 2023-07-25 | 畅的新材料科技（上海）有限公司 | Preparation method of modified nickel slurry for MLCC |
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| US4904411A (en) * | 1986-04-25 | 1990-02-27 | Ceramics Process Systems Corp. | Highly loaded, pourable suspensions of particulate materials |
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