CN114694898B - A kind of preparation method of MLCC nickel inner electrode slurry - Google Patents
A kind of preparation method of MLCC nickel inner electrode slurry Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 32
- 239000011267 electrode slurry Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 58
- 239000007900 aqueous suspension Substances 0.000 claims abstract description 52
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims abstract description 37
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229940116411 terpineol Drugs 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 32
- 239000000839 emulsion Substances 0.000 claims abstract description 32
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 26
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical group [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 18
- 239000010452 phosphate Substances 0.000 claims abstract description 18
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims abstract description 17
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims abstract description 17
- 239000000375 suspending agent Substances 0.000 claims abstract description 12
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 10
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 10
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 10
- 238000000967 suction filtration Methods 0.000 claims abstract description 10
- 239000000919 ceramic Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 8
- ZRGKYCBSAYCCTD-UAIGNFCESA-M sodium;(z)-but-2-enedioic acid;prop-2-enoate Chemical compound [Na+].[O-]C(=O)C=C.OC(=O)\C=C/C(O)=O ZRGKYCBSAYCCTD-UAIGNFCESA-M 0.000 claims description 6
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 5
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 4
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 4
- 229920005646 polycarboxylate Polymers 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 4
- PLLBRTOLHQQAQQ-UHFFFAOYSA-N 8-methylnonan-1-ol Chemical compound CC(C)CCCCCCCO PLLBRTOLHQQAQQ-UHFFFAOYSA-N 0.000 claims description 3
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- 229930195729 fatty acid Natural products 0.000 claims description 3
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- BVTJGGGYKAMDBN-UHFFFAOYSA-N Dioxetane Chemical compound C1COO1 BVTJGGGYKAMDBN-UHFFFAOYSA-N 0.000 claims 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims 1
- YQEMORVAKMFKLG-UHFFFAOYSA-N glycerine monostearate Natural products CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 claims 1
- SVUQHVRAGMNPLW-UHFFFAOYSA-N glycerol monostearate Natural products CCCCCCCCCCCCCCCCC(=O)OCC(O)CO SVUQHVRAGMNPLW-UHFFFAOYSA-N 0.000 claims 1
- 230000003746 surface roughness Effects 0.000 abstract description 13
- 239000006185 dispersion Substances 0.000 abstract description 11
- -1 phosphate ester Chemical class 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 9
- 239000002002 slurry Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 230000007774 longterm Effects 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 abstract description 2
- 230000002401 inhibitory effect Effects 0.000 abstract 1
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- 229940051841 polyoxyethylene ether Drugs 0.000 description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 description 12
- 238000012512 characterization method Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
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- 239000003990 capacitor Substances 0.000 description 2
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- 238000011056 performance test Methods 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229940075507 glyceryl monostearate Drugs 0.000 description 1
- 229940075529 glyceryl stearate Drugs 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 239000001788 mono and diglycerides of fatty acids Substances 0.000 description 1
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- 125000000542 sulfonic acid group Chemical group 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及电极浆料的制备方法，尤其是指一种MLCC镍内电极浆料的制备方法。The invention relates to a preparation method of electrode slurry, in particular to a preparation method of MLCC nickel inner electrode slurry.
背景技术Background technique
目前，超高容多层片式陶瓷电容器产品如0201X104、0201X105、0201X224、0402X106等使用的镍浆,要求镍粉粒径为0.3微米，钛酸钡粉粒径为0.1微米，粉体如此小的粒径对分散要求变得非常高。然而目前研究中大多数都将精力放在对镍粉的分散性上，而忽略陶瓷粉研究。MLCC用镍内电极浆料的制备方法主要是将金属粉研磨分散后与陶瓷粉和分散剂、粘结剂、有机溶剂混合搅拌，再用三辊轧机轧制。At present, the nickel paste used in ultra-high capacitance multilayer chip ceramic capacitor products such as 0201X104, 0201X105, 0201X224, 0402X106, etc., requires the particle size of nickel powder to be 0.3 microns, and the particle size of barium titanate powder to be 0.1 microns. The particle size becomes very demanding for dispersion. However, most of the current researches focus on the dispersibility of nickel powder, while ignoring the research on ceramic powder. The preparation method of nickel internal electrode slurry for MLCC is mainly to grind and disperse metal powder, mix and stir with ceramic powder, dispersant, binder and organic solvent, and then roll it with a three-roll mill.
此时浆料体系为悬浮液，长时间静置必然会发生分层，导致无机颗粒的团聚。又因镍粉比陶瓷粉粒径大，且分散剂一次性加入，分散剂往往与镍粉作用，不能充分作用于陶瓷粉，故分散效果欠佳。因此制备得到的镍浆中陶瓷粉更易团聚形成大颗粒，影响MLCC电容量。At this time, the slurry system is a suspension, and if it is left standing for a long time, stratification will inevitably occur, resulting in the agglomeration of inorganic particles. And because the nickel powder has a larger particle size than the ceramic powder, and the dispersant is added at one time, the dispersant often acts on the nickel powder and cannot fully act on the ceramic powder, so the dispersion effect is not good. Therefore, the ceramic powder in the prepared nickel slurry is more likely to agglomerate to form large particles, which affects the capacitance of the MLCC.
发明内容SUMMARY OF THE INVENTION
本发明正是为了克服上述不足，采用一种新的制备工艺来解决以上问题，创新点在于采用在浆料体系中形成乳液的形式来实现陶瓷粉在浆料中的高分散性，从而实现高电容量MLCC。In order to overcome the above-mentioned shortcomings, the present invention adopts a new preparation process to solve the above-mentioned problems. Capacitance MLCC.
具体是这样实施的：Specifically, it is implemented like this:
一种MLCC镍内电极浆料的制备方法，其特征在于工艺步骤如下：（1）将平均径100nm的BaTiO3粉末，水悬浮剂，去离子水，羟乙基纤维素混合，BaTiO3粉末、去离子水、羟乙基纤维素质量比为20：20：1，水悬浮剂占陶瓷粉质量的0.5%-2.5%，搅拌至少10min，乳化机3000转乳化30-60分钟至无大颗粒，得到BaTiO3的水悬浮液；A preparation method of MLCC nickel inner electrode slurry is characterized in that the process steps are as follows: ( 1 ) Mix BaTiO3 powder with an average diameter of 100 nm, water suspension agent, deionized water, hydroxyethyl cellulose, BaTiO3 powder, The mass ratio of deionized water and hydroxyethyl cellulose is 20:20:1, the water suspending agent accounts for 0.5%-2.5% of the mass of the ceramic powder, stir for at least 10min, and emulsify for 30-60 minutes at 3000 revolutions of the emulsifier until there are no large particles. Aqueous suspension of BaTiO 3 is obtained;
（2）将辛醇、松油醇、乙基纤维素按照质量比18：72：10混合，60℃机械搅拌5小时得到有机载体；(2) Mix octanol, terpineol, and ethyl cellulose according to a mass ratio of 18:72:10, and mechanically stir at 60°C for 5 hours to obtain an organic carrier;
（3）将步骤（1）制备的水悬浮液，步骤（2）制备的有机载体，平均径300nm的Ni粉，松油醇，乳化剂，磷酸酯分散剂NP-4混合，步骤（1）制备的水悬浮液、步骤（2）制备的有机载体、Ni粉、松油醇、磷酸酯分散剂NP-4质量比为18：20：50：11：1，乳化剂占步骤（1）制备的水悬浮液质量的1%-3%，自转公转搅拌机预混，再经三辊轧机研磨，直至钛酸钡的水悬浮液在松油醇体系中形成稳定的乳液液滴，得到钛酸钡乳液体系；(3) Mix the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder with an average diameter of 300 nm, terpineol, emulsifier, and phosphate dispersant NP-4, step (1) The mass ratio of the prepared aqueous suspension, the organic carrier prepared in step (2), Ni powder, terpineol, and phosphate dispersant NP-4 is 18:20:50:11:1, and the emulsifier accounts for the preparation in step (1). 1%-3% of the mass of the aqueous suspension of barium titanate, pre-mixed with a rotating revolution mixer, and then ground by a three-roll mill until the aqueous suspension of barium titanate forms stable emulsion droplets in the terpineol system to obtain barium titanate emulsion system;
（4）将步骤（3）制备的乳液进行抽滤，滤纸600目，得到镍内电极浆料。(4) Perform suction filtration on the emulsion prepared in step (3), filter paper 600 mesh, to obtain nickel inner electrode slurry.
本发明采用在浆料体系中形成陶瓷粉乳液的形式来实现陶瓷粉在浆料中的高分散性，首先采用水悬浮剂对陶瓷粉表面修饰，其吸附链锚定在陶瓷粉上，另一端亲水基团深入水相，通过粒子间静电斥力来稳定分散悬浮液。再通过乳化剂的亲水亲油特性，使得水悬浮液能够在有机溶剂中形成稳定的乳液，实现均匀分散。此方法最后形成稳定的乳液，相比常规的机械分散所形成的悬浮液，具有更均一的分散效果和长期稳定性。分散均匀不仅能充分发挥钛酸钡抑制收缩的能力，还能实现烧结后镍电极膜更小的表面粗糙度，使MLCC叠层数增加，获得更高的电容量。The invention adopts the form of forming a ceramic powder emulsion in a slurry system to realize the high dispersibility of the ceramic powder in the slurry. First, a water suspension agent is used to modify the surface of the ceramic powder, and its adsorption chain is anchored on the ceramic powder, and the other end is The hydrophilic group penetrates deep into the water phase and stabilizes the dispersion suspension through electrostatic repulsion between particles. Through the hydrophilic and lipophilic properties of the emulsifier, the aqueous suspension can form a stable emulsion in an organic solvent to achieve uniform dispersion. This method finally forms a stable emulsion with more uniform dispersion and long-term stability than suspensions formed by conventional mechanical dispersion. Uniform dispersion can not only give full play to the ability of barium titanate to suppress shrinkage, but also achieve a smaller surface roughness of the nickel electrode film after sintering, increase the number of MLCC stacks, and obtain higher capacitance.
进一步地，所述水悬浮剂为Tween80、马来酸-丙烯酸钠盐、木质素磺酸钙、异十醇聚氧乙烯醚、聚羧酸盐分散剂SD-819、木质素磺酸钠中的一种。羧基、磺酸基、聚氧化乙烯基等使分子具有梳形结构，水悬浮剂分子骨架由主链和较多的支链组成，主链上含有较多的活性基团，并且极性较强，依靠这些活性基团，主链可以“锚固”在陶瓷粉上，侧链具有亲水性，可以伸展在水中，在颗粒表面形成立体吸附结构，产生空间位阻效应，从而使陶瓷粉分散稳定。Further, the water suspending agent is Tween80, maleic acid-acrylic acid sodium salt, calcium lignosulfonate, isodecyl polyoxyethylene ether, polycarboxylate dispersant SD-819, sodium lignosulfonate. A sort of. Carboxyl group, sulfonic acid group, polyoxyethylene group, etc. make the molecule have a comb-shaped structure. The molecular skeleton of the aqueous suspension agent is composed of the main chain and more branched chains. The main chain contains more active groups and has strong polarity. , relying on these active groups, the main chain can be "anchored" on the ceramic powder, and the side chain is hydrophilic and can be stretched in water to form a three-dimensional adsorption structure on the surface of the particle, resulting in a steric hindrance effect, so that the ceramic powder can be dispersed stably .
进一步地，所述乳化剂为十二烷基硫酸钠（SDS）、单硬脂肪酸甘油酯、辛基酚聚氧乙烯醚（10）的一种。乳化剂中的亲油基、亲水基会***同性质的一侧，使其自身处于水-油界面处，最终形成乳化剂包裹水相均匀分布在油相里。Further, the emulsifier is one of sodium dodecyl sulfate (SDS), glyceryl monostearate, and octylphenol polyoxyethylene ether (10). The lipophilic and hydrophilic groups in the emulsifier will be inserted into the same side, so that they are located at the water-oil interface, and finally the emulsifier encapsulates the water phase and is evenly distributed in the oil phase.
本发明的有益效果是：在浆料体系中最后形成稳定的乳液，相比常规的机械分散所形成的悬浮液，具有更均一的分散效果和长期稳定性。分散均匀不仅能充分发挥钛酸钡抑制收缩的能力，还能实现烧结后镍电极膜更小的表面粗糙度，使MLCC叠层数增加，获得更高的电容量。The beneficial effects of the present invention are: a stable emulsion is finally formed in the slurry system, which has more uniform dispersion effect and long-term stability compared with the suspension formed by conventional mechanical dispersion. Uniform dispersion can not only give full play to the ability of barium titanate to suppress shrinkage, but also achieve a smaller surface roughness of the nickel electrode film after sintering, increase the number of MLCC stacks, and obtain higher capacitance.
附图说明Description of drawings
图1为对比例的表面粗糙度表征图。FIG. 1 is a surface roughness characterization diagram of a comparative example.
图2为实施例1的表面粗糙度表征图。FIG. 2 is a surface roughness characterization diagram of Example 1. FIG.
图3为实施例2的表面粗糙度表征图。FIG. 3 is a surface roughness characterization diagram of Example 2. FIG.
图4为实施例3的表面粗糙度表征图。FIG. 4 is a surface roughness characterization diagram of Example 3. FIG.
图5为实施例4的表面粗糙度表征图。FIG. 5 is a surface roughness characterization diagram of Example 4. FIG.
图6为实施例5的表面粗糙度表征图。FIG. 6 is a surface roughness characterization diagram of Example 5. FIG.
图7为实施例6的表面粗糙度表征图。FIG. 7 is a surface roughness characterization diagram of Example 6. FIG.
图8为对比例的SEM图。FIG. 8 is a SEM image of a comparative example.
图9为实施例1的SEM图。FIG. 9 is a SEM image of Example 1. FIG.
图10为实施例2的SEM图。FIG. 10 is an SEM image of Example 2. FIG.
图11为实施例3的SEM图。FIG. 11 is an SEM image of Example 3. FIG.
图12为实施例4的SEM图。FIG. 12 is an SEM image of Example 4. FIG.
图13为实施例5的SEM图。FIG. 13 is an SEM image of Example 5. FIG.
图14为实施例6的SEM图。FIG. 14 is an SEM image of Example 6. FIG.
具体实施方式Detailed ways
实施例1Example 1
一种MLCC镍内电极浆料的制备方法，工艺步骤如下：A preparation method of MLCC nickel inner electrode slurry, the process steps are as follows:
（1）将平均径100nm的BaTiO3粉末，水悬浮剂Tween80，去离子水，羟乙基纤维素混合，BaTiO3粉末、去离子水、羟乙基纤维素质量比为20：20：1，水悬浮剂Tween80占陶瓷粉质量的0.5%，搅拌至少10min，乳化机3000转乳化30分钟至无大颗粒，得到BaTiO3的水悬浮液；(1) Mix BaTiO 3 powder with an average diameter of 100nm, water suspension agent Tween80, deionized water, and hydroxyethyl cellulose. The mass ratio of BaTiO 3 powder, deionized water, and hydroxyethyl cellulose is 20:20:1, Aqueous suspension agent Tween80 accounts for 0.5% of the mass of the ceramic powder, stir for at least 10min, and emulsify for 30 minutes at 3000 revolutions of the emulsifier until there are no large particles to obtain a BaTiO3 water suspension;
（2）将辛醇、松油醇、乙基纤维素按照质量比18：72：10混合，60℃机械搅拌5小时得到有机载体；(2) Mix octanol, terpineol, and ethyl cellulose according to a mass ratio of 18:72:10, and mechanically stir at 60°C for 5 hours to obtain an organic carrier;
（3）将步骤（1）制备的水悬浮液，步骤（2）制备的有机载体，平均径300nm的Ni粉，松油醇，乳化剂十二烷基硫酸钠（SDS），磷酸酯分散剂NP-4混合，步骤（1）制备的水悬浮液、步骤（2）制备的有机载体、Ni粉、松油醇、磷酸酯分散剂NP-4质量比为18：20：50：11：1，乳化剂十二烷基硫酸钠（SDS）占步骤（1）制备的水悬浮液质量的1%，自转公转搅拌机预混，再经三辊轧机研磨10遍，直至钛酸钡的水悬浮液在松油醇体系中形成稳定的乳液液滴，得到钛酸钡乳液体系；(3) Combine the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder with an average diameter of 300 nm, terpineol, emulsifier sodium dodecyl sulfate (SDS), and phosphate dispersant. NP-4 is mixed, the mass ratio of the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder, terpineol, and phosphate dispersant NP-4 is 18:20:50:11:1 , the emulsifier sodium dodecyl sulfate (SDS) accounts for 1% of the mass of the aqueous suspension prepared in step (1), pre-mixed with a rotary revolution mixer, and then ground for 10 times by a three-roll mill until the aqueous suspension of barium titanate is In the terpineol system, stable emulsion droplets are formed to obtain a barium titanate emulsion system;
（4）将步骤（3）制备的乳液进行抽滤，滤纸600目，得到镍内电极浆料。(4) Perform suction filtration on the emulsion prepared in step (3), filter paper 600 mesh, to obtain nickel inner electrode slurry.
实施例2Example 2
一种MLCC镍内电极浆料的制备方法，工艺步骤如下：A preparation method of MLCC nickel inner electrode slurry, the process steps are as follows:
（1）将平均径100nm的BaTiO3粉末，水悬浮剂马来酸-丙烯酸钠盐，去离子水，羟乙基纤维素混合，BaTiO3粉末、去离子水、羟乙基纤维素质量比为20：20：1，水悬浮剂马来酸-丙烯酸钠盐占陶瓷粉质量的1.5%，搅拌15min，乳化机3000转乳化45分钟至无大颗粒，得到BaTiO3的水悬浮液；(1) Mix BaTiO 3 powder with an average diameter of 100nm, aqueous suspending agent maleic acid-sodium acrylate, deionized water, and hydroxyethyl cellulose. The mass ratio of BaTiO 3 powder, deionized water, and hydroxyethyl cellulose is 20:20:1, the aqueous suspending agent maleic acid-acrylic acid sodium salt accounts for 1.5% of the mass of the ceramic powder, stir for 15 minutes, and emulsifier at 3000 for 45 minutes until there are no large particles to obtain a BaTiO 3 water suspension;
（2）将辛醇、松油醇、乙基纤维素按照质量比18：72：10混合，60℃机械搅拌5小时得到有机载体；(2) Mix octanol, terpineol, and ethyl cellulose according to a mass ratio of 18:72:10, and mechanically stir at 60°C for 5 hours to obtain an organic carrier;
（3）将步骤（1）制备的水悬浮液，步骤（2）制备的有机载体，平均径300nm的Ni粉，松油醇，乳化剂单硬脂肪酸甘油酯，磷酸酯分散剂NP-4混合，步骤（1）制备的水悬浮液、步骤（2）制备的有机载体、Ni粉、松油醇、磷酸酯分散剂NP-4质量比为18：20：50：11：1，乳化剂单硬脂肪酸甘油酯占步骤（1）制备的水悬浮液质量的2%，自转公转搅拌机预混，再经三辊轧机研磨10遍，直至钛酸钡的水悬浮液在松油醇体系中形成稳定的乳液液滴，得到钛酸钡乳液体系；(3) Mix the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder with an average diameter of 300 nm, terpineol, emulsifier monostearic fatty acid glyceride, and phosphate dispersant NP-4. , the mass ratio of the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder, terpineol, and phosphate dispersant NP-4 is 18:20:50:11:1, and the emulsifier is single Glyceryl stearate accounts for 2% of the mass of the aqueous suspension prepared in step (1), premixed with a rotary revolution mixer, and then ground for 10 times by a three-roll mill until the aqueous suspension of barium titanate is stable in the terpineol system to obtain a barium titanate emulsion system;
（4）将步骤（3）制备的乳液进行抽滤，滤纸600目，得到镍内电极浆料。(4) Perform suction filtration on the emulsion prepared in step (3), filter paper 600 mesh, to obtain nickel inner electrode slurry.
实施例3Example 3
一种MLCC镍内电极浆料的制备方法，工艺步骤如下：A preparation method of MLCC nickel inner electrode slurry, the process steps are as follows:
（1）将平均径100nm的BaTiO3粉末，水悬浮剂木质素磺酸钙，去离子水，羟乙基纤维素混合，BaTiO3粉末、去离子水、羟乙基纤维素质量比为20：20：1，水悬浮剂木质素磺酸钙占陶瓷粉质量的2.5%，搅拌15min，乳化机3000转乳化60分钟至无大颗粒，得到BaTiO3的水悬浮液；(1) Mix BaTiO 3 powder with an average diameter of 100nm, calcium lignosulfonate as an aqueous suspension agent, deionized water, and hydroxyethyl cellulose. The mass ratio of BaTiO 3 powder, deionized water, and hydroxyethyl cellulose is 20: 20:1, the water suspension agent calcium lignosulfonate accounts for 2.5% of the mass of the ceramic powder, stir for 15 minutes, and emulsify for 60 minutes at 3000 revolutions of the emulsifier until there are no large particles to obtain a BaTiO 3 water suspension;
（2）将辛醇、松油醇、乙基纤维素按照质量比18：72：10混合，60℃机械搅拌5小时得到有机载体；(2) Mix octanol, terpineol, and ethyl cellulose according to a mass ratio of 18:72:10, and mechanically stir at 60°C for 5 hours to obtain an organic carrier;
（3）将步骤（1）制备的水悬浮液，步骤（2）制备的有机载体，平均径300nm的Ni粉，松油醇，乳化剂辛基酚聚氧乙烯醚（10），磷酸酯分散剂NP-4混合，步骤（1）制备的水悬浮液、步骤（2）制备的有机载体、Ni粉、松油醇、磷酸酯分散剂NP-4质量比为18：20：50：11：1，乳化剂辛基酚聚氧乙烯醚（10）占步骤（1）制备的水悬浮液质量的3%，自转公转搅拌机预混，再经三辊轧机研磨10遍，直至钛酸钡的水悬浮液在松油醇体系中形成稳定的乳液液滴，得到钛酸钡乳液体系；(3) Disperse the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder with an average diameter of 300 nm, terpineol, emulsifier octylphenol polyoxyethylene ether (10), and phosphate ester. Mixing agent NP-4, the mass ratio of the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder, terpineol, and phosphate dispersant NP-4 is 18:20:50:11: 1. The emulsifier octylphenol polyoxyethylene ether (10) accounts for 3% of the mass of the water suspension prepared in step (1). It is premixed with an autorotation and revolution mixer, and then ground for 10 times by a three-roll mill until the water of barium titanate is The suspension forms stable emulsion droplets in the terpineol system to obtain a barium titanate emulsion system;
（4）将步骤（3）制备的乳液进行抽滤，滤纸600目，得到镍内电极浆料。(4) Perform suction filtration on the emulsion prepared in step (3), filter paper 600 mesh, to obtain nickel inner electrode slurry.
实施例4Example 4
一种MLCC镍内电极浆料的制备方法，工艺步骤如下：A preparation method of MLCC nickel inner electrode slurry, the process steps are as follows:
（1）将平均径100nm的BaTiO3粉末，水悬浮剂异十醇聚氧乙烯醚，去离子水，羟乙基纤维素混合，BaTiO3粉末、去离子水、羟乙基纤维素质量比为20：20：1，水悬浮剂异十醇聚氧乙烯醚占陶瓷粉质量的1.5%，搅拌15min，乳化机3000转乳化45分钟至无大颗粒，得到BaTiO3的水悬浮液；(1) Mix BaTiO 3 powder with an average diameter of 100nm, water suspending agent isodecanol polyoxyethylene ether, deionized water, and hydroxyethyl cellulose. The mass ratio of BaTiO 3 powder, deionized water, and hydroxyethyl cellulose is 20:20:1, the water suspension agent isodecanol polyoxyethylene ether accounts for 1.5% of the mass of the ceramic powder, stir for 15 minutes, and emulsifier at 3000 rpm for 45 minutes until there are no large particles to obtain a BaTiO 3 water suspension;
（2）将辛醇、松油醇、乙基纤维素按照质量比18：72：10混合，60℃机械搅拌5小时得到有机载体；(2) Mix octanol, terpineol, and ethyl cellulose according to a mass ratio of 18:72:10, and mechanically stir at 60°C for 5 hours to obtain an organic carrier;
（3）将步骤（1）制备的水悬浮液，步骤（2）制备的有机载体，平均径300nm的Ni粉，松油醇，乳化剂辛基酚聚氧乙烯醚（10），磷酸酯分散剂NP-4混合，步骤（1）制备的水悬浮液、步骤（2）制备的有机载体、Ni粉、松油醇、磷酸酯分散剂NP-4质量比为18：20：50：11：1，乳化剂辛基酚聚氧乙烯醚（10）占步骤（1）制备的水悬浮液质量的2%，自转公转搅拌机预混，再经三辊轧机研磨15遍，直至钛酸钡的水悬浮液在松油醇体系中形成稳定的乳液液滴，得到钛酸钡乳液体系；(3) Disperse the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder with an average diameter of 300 nm, terpineol, emulsifier octylphenol polyoxyethylene ether (10), and phosphate ester. Mixing agent NP-4, the mass ratio of the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder, terpineol, and phosphate dispersant NP-4 is 18:20:50:11: 1. The emulsifier octylphenol polyoxyethylene ether (10) accounts for 2% of the mass of the aqueous suspension prepared in step (1). It is premixed with a rotary revolution mixer, and then ground for 15 times by a three-roll mill until the water of barium titanate is The suspension forms stable emulsion droplets in the terpineol system to obtain a barium titanate emulsion system;
（4）将步骤（3）制备的乳液进行抽滤，滤纸600目，得到镍内电极浆料。(4) Perform suction filtration on the emulsion prepared in step (3), filter paper 600 mesh, to obtain nickel inner electrode slurry.
实施例5Example 5
一种MLCC镍内电极浆料的制备方法，工艺步骤如下：A preparation method of MLCC nickel inner electrode slurry, the process steps are as follows:
（1）将平均径100nm的BaTiO3粉末，水悬浮剂聚羧酸盐分散剂SD-819，去离子水，羟乙基纤维素混合，BaTiO3粉末、去离子水、羟乙基纤维素质量比为20：20：1，水悬浮剂聚羧酸盐分散剂SD-819占陶瓷粉质量的1.5%，搅拌15min，乳化机3000转乳化45分钟至无大颗粒，得到BaTiO3的水悬浮液；(1) Mix BaTiO 3 powder with an average diameter of 100nm, water suspending agent polycarboxylate dispersant SD-819, deionized water, hydroxyethyl cellulose, BaTiO 3 powder, deionized water, hydroxyethyl cellulose mass The ratio is 20:20:1, the water suspending agent polycarboxylate dispersant SD-819 accounts for 1.5% of the mass of the ceramic powder, stirring for 15min, the emulsifier 3000 turns emulsification for 45 minutes until no large particles are obtained, and the water suspension of BaTiO3 is obtained ;
（2）将辛醇、松油醇、乙基纤维素按照质量比18：72：10混合，60℃机械搅拌5小时得到有机载体；(2) Mix octanol, terpineol, and ethyl cellulose according to a mass ratio of 18:72:10, and mechanically stir at 60°C for 5 hours to obtain an organic carrier;
（3）将步骤（1）制备的水悬浮液，步骤（2）制备的有机载体，平均径300nm的Ni粉，松油醇，乳化剂辛基酚聚氧乙烯醚（10），磷酸酯分散剂NP-4混合，步骤（1）制备的水悬浮液、步骤（2）制备的有机载体、Ni粉、松油醇、磷酸酯分散剂NP-4质量比为18：20：50：11：1，乳化剂辛基酚聚氧乙烯醚（10）占步骤（1）制备的水悬浮液质量的2%，自转公转搅拌机预混，再经三辊轧机研磨15遍，直至钛酸钡的水悬浮液在松油醇体系中形成稳定的乳液液滴，得到钛酸钡乳液体系；(3) Disperse the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder with an average diameter of 300 nm, terpineol, emulsifier octylphenol polyoxyethylene ether (10), and phosphate ester. Mixing agent NP-4, the mass ratio of the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder, terpineol, and phosphate dispersant NP-4 is 18:20:50:11: 1. The emulsifier octylphenol polyoxyethylene ether (10) accounts for 2% of the mass of the aqueous suspension prepared in step (1). It is premixed with a rotary revolution mixer, and then ground for 15 times by a three-roll mill until the water of barium titanate is The suspension forms stable emulsion droplets in the terpineol system to obtain a barium titanate emulsion system;
（4）将步骤（3）制备的乳液进行抽滤，滤纸600目，得到镍内电极浆料。(4) Perform suction filtration on the emulsion prepared in step (3), filter paper 600 mesh, to obtain nickel inner electrode slurry.
实施例6Example 6
一种MLCC镍内电极浆料的制备方法，工艺步骤如下：A preparation method of MLCC nickel inner electrode slurry, the process steps are as follows:
（1）将平均径100nm的BaTiO3粉末，水悬浮剂木质素磺酸钠，去离子水，羟乙基纤维素混合，BaTiO3粉末、去离子水、羟乙基纤维素质量比为20：20：1，水悬浮剂木质素磺酸钠占陶瓷粉质量的1.5%，搅拌15min，乳化机3000转乳化45分钟至无大颗粒，得到BaTiO3的水悬浮液；(1) Mix BaTiO 3 powder with an average diameter of 100nm, water suspending agent sodium lignosulfonate, deionized water, and hydroxyethyl cellulose. The mass ratio of BaTiO 3 powder, deionized water, and hydroxyethyl cellulose is 20: 20:1, the water suspending agent sodium lignosulfonate accounts for 1.5% of the mass of the ceramic powder, stir for 15 minutes, and emulsify at 3000 revolutions of the emulsifier for 45 minutes until there are no large particles, to obtain an aqueous suspension of BaTiO 3 ;
（2）将辛醇、松油醇、乙基纤维素按照质量比18：72：10混合，60℃机械搅拌5小时得到有机载体；(2) Mix octanol, terpineol, and ethyl cellulose according to a mass ratio of 18:72:10, and mechanically stir at 60°C for 5 hours to obtain an organic carrier;
（3）将步骤（1）制备的水悬浮液，步骤（2）制备的有机载体，平均径300nm的Ni粉，松油醇，乳化剂辛基酚聚氧乙烯醚（10），磷酸酯分散剂NP-4混合，步骤（1）制备的水悬浮液、步骤（2）制备的有机载体、Ni粉、松油醇、磷酸酯分散剂NP-4质量比为18：20：50：11：1，乳化剂辛基酚聚氧乙烯醚（10）占步骤（1）制备的水悬浮液质量的2%，自转公转搅拌机预混，再经三辊轧机研磨15遍，直至钛酸钡的水悬浮液在松油醇体系中形成稳定的乳液液滴，得到钛酸钡乳液体系；(3) Disperse the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder with an average diameter of 300 nm, terpineol, emulsifier octylphenol polyoxyethylene ether (10), and phosphate ester. Mixing agent NP-4, the mass ratio of the aqueous suspension prepared in step (1), the organic carrier prepared in step (2), Ni powder, terpineol, and phosphate dispersant NP-4 is 18:20:50:11: 1. The emulsifier octylphenol polyoxyethylene ether (10) accounts for 2% of the mass of the aqueous suspension prepared in step (1). It is premixed with a rotary revolution mixer, and then ground for 15 times by a three-roll mill until the water of barium titanate is The suspension forms stable emulsion droplets in the terpineol system to obtain a barium titanate emulsion system;
（4）将步骤（3）制备的乳液进行抽滤，滤纸600目，得到镍内电极浆料。(4) Perform suction filtration on the emulsion prepared in step (3), filter paper 600 mesh, to obtain nickel inner electrode slurry.
对比例Comparative ratio
（1）将辛醇，松油醇，乙基纤维素按照质量比18：72：10混合，60℃机械搅拌5小时得到有机载体。(1) Mix octanol, terpineol, and ethyl cellulose according to a mass ratio of 18:72:10, and mechanically stir at 60°C for 5 hours to obtain an organic carrier.
（2）采用传统制备方法将平均径300nm的Ni粉，平均径100nm的BaTiO3粉末，（1）制备的有机载体，松油醇，磷酸酯分散剂NP-4按照质量比50：12.5：25：11：1.5混合，搅拌均匀，自转公转搅拌机预混，再经三辊轧机研磨15遍。(2) Ni powder with an average diameter of 300 nm, BaTiO3 powder with an average diameter of 100 nm, organic carrier prepared in (1), terpineol, and phosphate ester dispersant NP-4 were prepared according to the mass ratio of 50:12.5:25: 11:1.5 mixing, stirring evenly, pre-mixing with a rotating and revolving mixer, and then grinding for 15 times by a three-roll mill.
（3）将（2）制备的浆料进行抽滤，滤纸600目，得到镍内电极浆料。(3) The slurry prepared in (2) is subjected to suction filtration, and the filter paper is 600 mesh to obtain the nickel inner electrode slurry.
对实施例1-6，对比例制得的镍内电极浆料进行表面粗糙度Rp检测（参见图1-图7）、SEM表征检测（参见图8-14）、电性能测试(参见表1)。Surface roughness Rp detection (see Figure 1-Figure 7), SEM characterization detection (see Figure 8-14), and electrical performance test (see Table 1) were performed on the nickel internal electrode pastes prepared in Examples 1-6 and Comparative Examples. ).
电性能测试采用四参数测试机，能够同时测试MLCC的容值、损耗、绝缘电阻及耐电压，测试电压1V，频率1KHZ。针对0603X105K250NBH的MLCC电容器，其电性能要求为：容值允许范围为0.9~1.1μF，损耗DF≤3 .5%，耐电压BV≥62 .5V，绝缘电阻IR×C≥100s。测试数据见表1。The electrical performance test adopts a four-parameter testing machine, which can simultaneously test the capacitance, loss, insulation resistance and withstand voltage of the MLCC. The test voltage is 1V and the frequency is 1KHZ. For the MLCC capacitor of 0603X105K250NBH, its electrical performance requirements are: the allowable range of capacitance is 0.9~1.1μF, the loss DF≤3.5%, the withstand voltage BV≥62.5V, and the insulation resistance IR×C≥100s. The test data are shown in Table 1.
备注：表中，容值、损耗及绝缘电阻为50粒MLCC成品电容器的平均值，耐电压为范围值。Remarks: In the table, the capacitance, loss and insulation resistance are the average values of 50 MLCC finished capacitors, and the withstand voltage is the range value.
从图1-图7所示，各实施例的表面粗糙度相比对比例有较大改善，仅为对比例的36%-64%，表面粗糙度较小，意味着MLCC能够叠层数量更多，电容量更高。As shown in Figures 1 to 7, the surface roughness of each embodiment is greatly improved compared to the comparative example, which is only 36%-64% of the comparative example, and the surface roughness is small, which means that the number of MLCC layers can be increased. more, the higher the capacity.
通过图8-14的SEM表征图，各实施例的颗粒分布均匀，无明显团聚，对比对比例有明显提升。According to the SEM characterization diagrams in Figs. 8-14, the particles of each example are uniformly distributed, and there is no obvious agglomeration, which is significantly improved compared to the comparative examples.
从表1的电性能表征，可知各实施例的参数相比对比例提升效果明显，能够获得更高的电容量，更小的损耗，更高的耐电压。From the electrical performance characterization in Table 1, it can be seen that the parameters of each embodiment are significantly improved compared to the comparative example, and higher capacitance, smaller loss, and higher withstand voltage can be obtained.
本发明各实施例中，实施例2为最优配比。Among the various embodiments of the present invention, Example 2 is the optimal ratio.
Claims (5)
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| CN112368786A (en) * | 2018-09-28 | 2021-02-12 | 住友金属矿山株式会社 | Conductive paste, electronic component, and multilayer ceramic capacitor |
| CN113948235A (en) * | 2021-12-20 | 2022-01-18 | 西安宏星电子浆料科技股份有限公司 | High-dispersity low-shrinkage nickel inner electrode slurry and preparation method thereof |
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| US6268054B1 (en) * | 1997-02-18 | 2001-07-31 | Cabot Corporation | Dispersible, metal oxide-coated, barium titanate materials |
| JP2004200449A (en) * | 2002-12-19 | 2004-07-15 | Sumitomo Metal Mining Co Ltd | Conductive paste composition for internal electrode of multilayer ceramic capacitor |
| WO2006098091A1 (en) * | 2005-03-14 | 2006-09-21 | Murata Manufacturing Co., Ltd. | Dispersion apparatus, process for producing ceramic slurry, laminated ceramic electronic component and process for producing the same |
| CN100485835C (en) * | 2006-03-10 | 2009-05-06 | 潮州三环（集团）股份有限公司 | Inner electrode size of ceramic capacitor and preparation method thereof |
| US20100110608A1 (en) * | 2008-11-06 | 2010-05-06 | Frank Wei | Core-shell structured dielectric particles for use in multilayer ceramic capacitors |
| CN101913863B (en) * | 2010-07-23 | 2013-07-03 | 广东风华高新科技股份有限公司 | Ceramic dielectric material matched with nickel inner electrode |
| CN102211206B (en) * | 2011-05-25 | 2013-09-18 | 华东微电子技术研究所合肥圣达实业公司 | Method for preparing superfine spherical silver powder for barium-titanate-based semiconductor ceramic ohmic electrode slurry |
| CN102327806B (en) * | 2011-06-20 | 2014-03-26 | 宁波广博纳米新材料股份有限公司 | Method taking organic solvent as medium for grading nano-nickel powder for MLCC (multilayer ceramic capacitor) |
| CN102683034B (en) * | 2012-04-28 | 2015-03-25 | 中国科学院电工研究所 | Method for preparing super capacitor electrode plate |
| CN109467931B (en) * | 2017-09-07 | 2020-10-02 | 北京化工大学 | A kind of flexible dielectric elastomer composite material based on nano liquid metal and preparation method thereof |
| CN112768234B (en) * | 2020-12-28 | 2021-09-24 | 潮州三环（集团）股份有限公司 | Nickel electrode slurry and preparation method and application thereof |
| CN112992431B (en) * | 2021-04-16 | 2021-08-03 | 西安宏星电子浆料科技股份有限公司 | High-dispersion nickel inner electrode slurry for multilayer chip ceramic capacitor and preparation method thereof |
| CN113823437B (en) * | 2021-09-28 | 2023-02-14 | 大连海外华昇电子科技有限公司 | Roll printing slurry for MLCC gravure printing process and preparation process thereof |
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| CN112368786A (en) * | 2018-09-28 | 2021-02-12 | 住友金属矿山株式会社 | Conductive paste, electronic component, and multilayer ceramic capacitor |
| CN113948235A (en) * | 2021-12-20 | 2022-01-18 | 西安宏星电子浆料科技股份有限公司 | High-dispersity low-shrinkage nickel inner electrode slurry and preparation method thereof |
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