CN104174841A - Production method of nickel paste for ultrahigh-capacitance MLCC (multilayer ceramic capacitor), nickel paste and MLCC - Google Patents
Production method of nickel paste for ultrahigh-capacitance MLCC (multilayer ceramic capacitor), nickel paste and MLCC Download PDFInfo
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- CN104174841A CN104174841A CN201410407267.2A CN201410407267A CN104174841A CN 104174841 A CN104174841 A CN 104174841A CN 201410407267 A CN201410407267 A CN 201410407267A CN 104174841 A CN104174841 A CN 104174841A
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Abstract
The invention discloses a production method of nickel paste for an ultrahigh-capacitance MLCC (multilayer ceramic capacitor). The production method includes the steps of 1, dispersing nickel powder, dispersant and solvent with a sander; 2, dispersing barium titanate powder, dispersant and solvent with the sander; 3, mixing a product of the first step and a product of the second step, and performing mixing before adding adhesive; 4, performing conventional dispersion and filtration. The invention further provides nickel paste produced by the production method of the nickel paste for the ultrahigh-capacitance MLCC and an MLCC produced with the nickel paste for the ultrahigh-capacitance MLCC. The production method has the advantages that nickel powder and barium titanate powder can be dispersed more effectively, and the produced MLCC is good in voltage resistance and HALT (highly accelerated life testing) performance.
Description
Technical field
The present invention relates to superelevation and hold the preparation method of nickel slurry for MLCC, particularly superelevation is held the process for dispersing of nickel slurry for MLCC.The invention still further relates to by superelevation appearance MLCC and starch with the nickel that the preparation method that nickel is starched obtains, and the MLCC being made by this nickel slurry.
Background technology
At present, superelevation is held the nickel slurry that multiple-layer sheet ceramic capacitor (MLCC) product is used as 0402X5R225,0805X5R226 etc., and requiring nickel powder particle diameter is 0.17～0.20 μ m, and barium titanate powder particle diameter is 0.05～0.1 μ m.The particle diameter that powder is so little requires to become very high to disperseing.If dispersion effect is bad, in nickel slurry, exist the bulky grain of reuniting can cause that product is withstand voltage, Highly Accelerated Life Test (HALT) performance worsens, even cause scrapping.
The general technology flow process that nickel slurry is made is at present: nickel powder, barium titanate powder and dispersant, adhesive, solvent are mixed together after stirring, then with three-high mill, roll slurry and disperse.The height of making like this holds nickel slurry and does not often reach the dispersion effect needing, and makes that product is withstand voltage, HALT poor performance.
The nickel slurry dispersing technology of prior art stirs nickel powder, through milling train, disperses together with barium titanate powder, but in fact nickel powder and barium titanate powder particle diameter different, disperse to require also different, when both are disperseed together, cannot guarantee that two kinds of powders all disperse completely simultaneously.The present invention after nickel powder and barium titanate powder are disperseed with sand mill respectively again mix and blend, together with roll slurry, effectively improved the dispersion effect of powder.The nickel slurry good dispersion being made by preparation method of the present invention, can meet the requirement that preparation superelevation is held MLCC.The MLCC product electrical property that utilizes nickel slurry of the present invention to make is excellent, and particularly withstand voltage properties is good, and HALT performance has significant lifting with respect to prior art products.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of superelevation and hold the preparation method of nickel slurry for MLCC, the technical scheme adopting is:
Superelevation is held the preparation method of nickel slurry for MLCC, comprises the following steps:
(1) get nickel powder, dispersant and solvent, with sand mill, disperse;
(2) get barium titanate powder, dispersant and solvent, with sand mill, disperse;
(3) by step (1), (2) gained mixing of materials, add adhesive to stir;
(4) conventional dispersion, filtration.
Preferably, be dispersed under 1500-2500rpm described in step (1), (2) and carry out, more preferably, disperse 2 ± 0.5h.
Preferably, in step (1), the addition of nickel powder is the 40-70% of step (1) material gross weight, the 0.3-2% that the addition of dispersant is 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 0.3-2% that the addition of dispersant is gross weight, and surplus is solvent.
Preferably, dispersant described in step (1), (2) be that phosphoric acid ester dispersant, sapn series, polycarboxylic acids are serial, one or more in lecithin etc.
Preferably, solvent described in step (1), (2) is one or more in dodecane, dibutyl phthalate, dioctyl phthalate, octanol, terpinol, phenmethylol, diethylene glycol monobutyl ether, menthol.
Preferably, the described adhesive of step (3) is that concentration is 8～20% ethyl cellulose solution.Preferably, by one or more dissolvings in solvent dodecane, dibutyl phthalate, dioctyl phthalate, octanol, terpinol, phenmethylol, diethylene glycol monobutyl ether, menthol for ethyl cellulose resin, make ethyl cellulose concentration (w/v) for 8-20%, make adhesive.
Preferably, identical solvent is used in step (1) and (2).Preferably, the solvent phase that in step (3), the solvent of preparation adhesive and step (1) and/or (2) are used is same.More preferably, identical solvent is used in step (1) and (2), and in step (3), the solvent of preparation adhesive is also same with the solvent phase that step (1) and (2) are used.
Preferably, the ratio of step (1) material gross weight, step (2) material gross weight and the described binder wt of step (3) is 100:(10-30): (20-40).
Preferably, the described routine of step (4) is separated into and adopts three-high mill to carry out grinding distribution, more preferably, disperses 5 ± 0.5h.
Preferably, by filter core, carry out secondary filter after being filtered into dilution described in step (4).
The present invention also provides a kind of superelevation of using to hold the nickel slurry that MLCC obtains by the preparation method that nickel is starched.
In addition, the present invention also provides a kind of MLCC being made with nickel slurry by superelevation appearance MLCC.Preparation method is identical with the method that common nickel slurry is prepared MLCC.
The invention has the beneficial effects as follows:
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of nickel powder before disperseing;
Fig. 2 is the SEM figure of nickel slurry after embodiment 1 disperses;
Fig. 3 is the SEM figure of nickel slurry after embodiment 2 disperses;
Fig. 4 is the SEM figure of nickel slurry after embodiment 3 disperses.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.Following examples, for for example, are not only limitation of the present invention.Equal replacement, modification or the change on basis of the present invention, made, all fall within the scope of protection of the present invention.
Embodiment 1
Making by the following method superelevation appearance MLCC starches with nickel:
(1) get by weight the nickel powder of 40 parts, the phosphoric acid ester dispersant Hostaphat OPS 75E of 0.3 part and the dodecane of 59.7 parts, be placed in sand mill, in 1500rpm, disperse 2 hours.
(2) get by weight the barium titanate powder of 40 parts, 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 10% of step (1) material gross weight.Material is placed in to sand mill, in 1500rpm, disperses 2 hours.
(3) by the mixing of materials of step (1) and (2), and add adhesive to stir; Wherein the preparation method of adhesive is: ethyl cellulose resin is dissolved with dodecane, and making the concentration (w/v) of ethyl cellulose is 8%.The addition of adhesive is 20% of step (1) material gross weight.
(4) use three-high mill grinding distribution 5 hours.
(5) after dilution, by filter core, carry out secondary filter, thoroughly remove bulky grain.
Embodiment 2
Making by the following method superelevation appearance MLCC starches with nickel:
(1) get by weight the nickel powder, the phosphoric acid ester dispersant Hostaphat OPS 75E of 0.5 part, 0.5 part of sapn Series Dispersant S-40, the octanol of 22 parts, the terpinol of 22 parts of 55 parts, be placed in sand mill, in 2000rpm, disperse 2.5 hours.
(2) get by weight the barium titanate powder, the phosphoric acid ester dispersant Hostaphat OPS75E of 0.5 part, 0.5 part of sapn Series Dispersant S-40, the octanol of 24 parts, the terpinol of 24 parts of 51 parts; Material gross weight is herein 20% of step (1) material gross weight.Material is placed in to sand mill, in 2000rpm, disperses 2.5 hours.
(3) by the mixing of materials of step (1) and (2), and add adhesive to stir; Wherein the preparation method of adhesive is: ethyl cellulose resin is dissolved with octanol, and making the concentration (w/v) of ethyl cellulose is 15%.The addition of adhesive is 30% of step (1) material gross weight.
(4) use three-high mill grinding distribution 5.5 hours.
(5) after dilution, by filter core, carry out secondary filter, thoroughly remove bulky grain.
Embodiment 3
Making by the following method superelevation appearance MLCC starches with nickel:
(1) get by weight the nickel powder of 70 parts, 2 parts of lecithin, 28 parts of menthols, be placed in sand mill, in 2500rpm, disperse 1.5 hours.
(2) get by weight the barium titanate powder of 70 parts, 2 parts of lecithin, 28 parts of menthols; The gross weight of barium titanate powder, lecithin and menthol is 30% of step (1) material gross weight.Material is placed in to sand mill, in 2500rpm, disperses 1.5 hours.
(3) by the mixing of materials of step (1) and (2), and add adhesive to stir; Wherein the preparation method of adhesive is: ethyl cellulose resin is dissolved with menthol, and making the concentration (w/v) of ethyl cellulose is 20%.The addition of adhesive is 40% of step (1) material gross weight.
(4) use three-high mill grinding distribution 4.5 hours.
(5) after dilution, by filter core, carry out secondary filter, thoroughly remove bulky grain.
Embodiment 4
Get the nickel slurry after nickel powder before dispersion and embodiment 1-3 disperse, under SEM, observe.Result as shown in Figure 1, Figure 2, Figure 3 and Figure 4.Fig. 1 is the SEM figure of the nickel powder before disperseing, and Fig. 2-4 are respectively the SEM figure of the nickel slurry after embodiment 1,2,3 disperses.SEM figure contrast from Fig. 2-4 with Fig. 1, in embodiment of the present invention 1-3, nickel powder and barium titanate powder disperse completely, and nickel slurry dispersion effect is good.
Embodiment 5
Get the nickel that nickel is starched and prepared by prior art slurry prepared by embodiment 1-3, according to conventional method, respectively make 80 (0402X5R105) MLCC products, test under the same conditions the electrical property of all products.Wherein, nickel slurry prepared by prior art refers to nickel powder, barium titanate powder and dispersant, adhesive, solvent is mixed together after stirring, then rolls and starch the nickel slurry that disperses and obtain with three-high mill.Test result is as shown in table 1:
Table 1 embodiment 1-3 and prior art nickel slurry make 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, and Halt is Highly Accelerated Life Test.From table 1, with respect to the MLCC of prior art nickel slurry preparation, the Cp of the MLCC of the nickel slurry preparation of embodiment of the present invention 1-3 is large, BDV is higher, and HALT performance has remarkable lifting, and the electrical property of product is excellent.
Claims (10)
1. superelevation is held the preparation method of nickel slurry for MLCC, comprises the following steps:
(1) get nickel powder, dispersant and solvent, with sand mill, disperse;
(2) get barium titanate powder, dispersant and solvent, with sand mill, disperse;
(3) by step (1), (2) gained mixing of materials, add adhesive to stir;
(4) conventional dispersion, filtration.
2. superelevation according to claim 1 is held the preparation method of nickel slurry for MLCC, it is characterized in that: step (1), (2) described dispersion are to disperse 2 ± 0.5h under 1500-2500rpm.
3. superelevation according to claim 1 is held the preparation method of nickel slurry for MLCC, it is characterized in that: in step (1), the addition of nickel powder is the 40-70% of step (1) material gross weight, the 0.3-2% that the addition of dispersant is gross weight, and surplus is solvent.
4. superelevation according to claim 1 is held the preparation method of nickel slurry for MLCC, it is characterized in that: in step (2), the addition of barium titanate powder is the 40-70% of step (2) material gross weight, the 0.3-2% that the addition of dispersant is gross weight, and surplus is solvent.
5. superelevation according to claim 1 is held the preparation method of nickel slurry for MLCC, it is characterized in that: dispersant described in step (1), (2) is that phosphoric acid ester dispersant, sapn series, polycarboxylic acids are serial, one or more in lecithin.
6. superelevation according to claim 1 is held the preparation method of nickel slurry for MLCC, it is characterized in that: solvent described in step (1), (2) is one or more in dodecane, dibutyl phthalate, dioctyl phthalate, octanol, terpinol, phenmethylol, diethylene glycol monobutyl ether, menthol.
7. superelevation according to claim 1 is held the preparation method of nickel slurry for MLCC, it is characterized in that: the described adhesive of step (3) is that concentration is 8～20% ethyl cellulose solution.
8. superelevation according to claim 1 is held the preparation method of nickel slurry for MLCC, it is characterized in that: the ratio of step (1) material gross weight, step (2) material gross weight and step (3) binder wt is 100:(10-30): (20-40).
9. one kind is used superelevation to hold the nickel slurry that MLCC obtains by the preparation method that nickel is starched.
10. one kind is held by superelevation the MLCC that MLCC makes with nickel slurry.
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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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN116313512A (en) * | 2023-05-19 | 2023-06-23 | 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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Cited By (3)
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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 |
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