JP2005104782A - Slurry, green sheet, stacked electronic component and their manufacturing methods - Google Patents
Slurry, green sheet, stacked electronic component and their manufacturing methods Download PDFInfo
- Publication number
- JP2005104782A JP2005104782A JP2003341306A JP2003341306A JP2005104782A JP 2005104782 A JP2005104782 A JP 2005104782A JP 2003341306 A JP2003341306 A JP 2003341306A JP 2003341306 A JP2003341306 A JP 2003341306A JP 2005104782 A JP2005104782 A JP 2005104782A
- Authority
- JP
- Japan
- Prior art keywords
- additive
- slurry
- green sheet
- producing
- binder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002002 slurry Substances 0.000 title claims abstract description 61
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 49
- 239000000654 additive Substances 0.000 claims abstract description 88
- 230000000996 additive effect Effects 0.000 claims abstract description 82
- 239000000843 powder Substances 0.000 claims abstract description 38
- 239000011230 binding agent Substances 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 238000010298 pulverizing process Methods 0.000 claims description 41
- 239000002245 particle Substances 0.000 claims description 40
- 238000002360 preparation method Methods 0.000 claims description 11
- 238000010030 laminating Methods 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 4
- 150000004706 metal oxides Chemical class 0.000 abstract description 4
- 238000001238 wet grinding Methods 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 description 17
- 238000001035 drying Methods 0.000 description 16
- 239000003985 ceramic capacitor Substances 0.000 description 14
- 238000002156 mixing Methods 0.000 description 14
- 239000003960 organic solvent Substances 0.000 description 14
- 239000011362 coarse particle Substances 0.000 description 13
- 238000004220 aggregation Methods 0.000 description 12
- 238000001354 calcination Methods 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 230000002776 aggregation Effects 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052788 barium Inorganic materials 0.000 description 4
- -1 polyethylene terephthalate Polymers 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000007606 doctor blade method Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000002003 electrode paste Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Abstract
Description
本発明は、スラリー、グリーンシート及び積層型電子部品ならびにこれらの製造方法に関する。 The present invention relates to a slurry, a green sheet, a multilayer electronic component, and a method for producing them.
積層セラミックコンデンサ、積層型バリスタ、チップインダクタ等の積層型電子部品は、通常、セラミックスラリーを用いて形成されたセラミックグリーンシートを積層、圧着し、熱処理して、所定サイズに切断後、焼結工程を経て製造される。 Multilayer electronic components such as multilayer ceramic capacitors, multilayer varistors, and chip inductors are usually laminated with a ceramic green sheet formed using ceramic slurry, crimped, heat treated, cut into a predetermined size, and then sintered. It is manufactured through.
例えば、積層セラミックコンデンサは、以下のような方法で製造される。図３に積層セラミックコンデンサの製造工程を示す。まず、金属酸化物等の原料を秤量して調合を行い（ステップＳ５１）、ボールミル等で混合・粉砕し（ステップＳ５２）、その後、乾燥（ステップＳ５３）、仮焼き（ステップＳ５４）を行うことにより、添加剤を完成させる（ステップＳ５５）。次に、例えば、水を加えて再度ボールミル等で湿式粉砕（ステップＳ５６）を行い、乾燥（ステップＳ５７）を行った後、有機溶剤等を加えて予備粉砕を行う（ステップＳ５８）。続いて、予備粉砕された添加剤と誘電体粉末とを秤量して調合を行い、有機溶剤、有機バインダー等を加えてボールミル等で湿式粉砕（ステップＳ５９）を行うことにより、セラミックスラリーを製造する（ステップＳ６０）。 For example, a multilayer ceramic capacitor is manufactured by the following method. FIG. 3 shows a manufacturing process of the multilayer ceramic capacitor. First, raw materials such as metal oxides are weighed and prepared (step S51), mixed and pulverized with a ball mill or the like (step S52), and then dried (step S53) and calcined (step S54). The additive is completed (step S55). Next, for example, water is added and wet pulverization is performed again with a ball mill or the like (step S56), and after drying (step S57), an organic solvent or the like is added and preliminary pulverization is performed (step S58). Subsequently, the pre-ground additive and dielectric powder are weighed and prepared, and an organic solvent, an organic binder, etc. are added, and wet pulverization is performed with a ball mill or the like (step S59), thereby producing a ceramic slurry. (Step S60).
次に、製造されたセラミックスラリーをドクターブレード法、ノズル法などを用いてポリエチレンテレフタレート（ＰＥＴ）フィルム等の支持体上に塗布し、溶剤を乾燥させて、セラミックグリーンシートを製造する（ステップＳ６１）。続いて、支持体からセラミックグリーンシートを剥離し、これを複数枚積層し、圧着（ステップＳ６２）した後、所定のサイズに切断してグリーンチップとする。これらのグリーンチップの有機バインダー、可塑剤等を熱処理等で除去した後、焼成、外部電極形成等の処理を施すことにより積層セラミックコンデンサを製造する（ステップＳ６３）。 Next, the produced ceramic slurry is applied onto a support such as a polyethylene terephthalate (PET) film using a doctor blade method, a nozzle method, etc., and the solvent is dried to produce a ceramic green sheet (step S61). . Subsequently, the ceramic green sheets are peeled off from the support, and a plurality of these are laminated, pressure-bonded (step S62), and then cut into a predetermined size to obtain a green chip. After removing the organic binder, plasticizer, and the like of these green chips by heat treatment or the like, a multilayer ceramic capacitor is manufactured by performing processes such as firing and external electrode formation (step S63).
ところで、近年、積層型電子部品に対しては、小型化、高性能化が求められるようになっている。このため、積層型電子部品の製造に用いられるグリーンシートの層構造には、薄さとともに、高い均一性が求められるようになっている。例えば、塗膜時の塗布ムラ、成分不均一などのわずかのシート欠陥であっても、これが電子部品電気特性や信頼性に与える影響が無視できないレベルとなっている。このような状況下で誘電体層中の添加剤の分散が不均一であると、積層型電子部品の温度特性、品質、信頼性等が著しく低下してしまう。このため、誘電体粉末（主剤）に対して添加剤が均一に分散するように、添加剤の分散性を向上させる必要がある。 Incidentally, in recent years, there has been a demand for miniaturization and high performance for multilayer electronic components. For this reason, the green sheet layer structure used in the manufacture of multilayer electronic components is required to have high uniformity as well as thinness. For example, even a slight sheet defect such as coating unevenness or non-uniform component at the time of coating is at a level where the influence of this on electronic component electrical characteristics and reliability cannot be ignored. Under such circumstances, if the dispersion of the additive in the dielectric layer is not uniform, the temperature characteristics, quality, reliability, etc. of the multilayer electronic component will be significantly reduced. For this reason, it is necessary to improve the dispersibility of the additive so that the additive is uniformly dispersed in the dielectric powder (main agent).
添加剤の分散性を向上させる方法として、例えば、セラミック主成分粉末のメジアン値を５μｍ以下とし、添加剤として、メジアン値が１／５以下のものを使用し、添加剤の混合方法として、セラミックスラリー中に添加剤塩の水溶液を加えて混合し、スラリーを乾燥し、セラミック粒子を析出させる方法が提案されている（例えば、特許文献１参照）。
特許文献１では、添加剤を溶液として主成分粉末に加えて混合し、熱処理しているため、添加する金属の溶液を液体で秤量する必要があり、スラリー製造工程における作業数が増えたり、ｐＨ制御を行ったりしなくてはならない。このため、容易にスラリーを製造することができず、グリーンシート及び積層型電子部品を容易に製造することができなかった。
In
また、添加する金属を溶液状態で保存することになるため、酸化などの劣化が起こりやすく、保存しにくい形態であった。また、溶液を用いるので、コストも高くなってしまう。 In addition, since the metal to be added is stored in a solution state, deterioration such as oxidation is likely to occur and it is difficult to store. Moreover, since a solution is used, cost will also become high.
さらに、図３に示すような従来の製造方法では、添加剤のボールミル等での湿式粉砕、乾燥の工程が多いため、粉砕が進み細粒化が進めば、乾燥後の凝集力も大きくなり、乾燥後のボールミル等での湿式粉砕で凝集体の粉砕が進まずに、粗粒子が生じやすくなってしまう。このような粗粒子が、グリーンシート製造時に混入してしまうと、品質、信頼性等が低下する不良を引き起こす事になる。さらに、添加剤の細粒化が進んでいるので、添加剤と主剤との混合時に再凝集が生じてしまうおそれもある。 Furthermore, in the conventional manufacturing method as shown in FIG. 3, since there are many wet pulverization and drying steps in a ball mill or the like of the additive, if the pulverization proceeds and the finer granulation progresses, the cohesive force after drying increases, and the drying In the subsequent wet pulverization with a ball mill or the like, the pulverization of the agglomerates does not proceed, and coarse particles are easily generated. If such coarse particles are mixed during the production of the green sheet, the quality, reliability and the like are deteriorated. Furthermore, since the additive is becoming finer, re-aggregation may occur when the additive and the main agent are mixed.
また、特許文献１には、主成分の平均粒径が２．３〜５．１μｍのものが記載されており、例えば、粒径が２μｍを超える主成分粒子を用いる場合、誘電体層の厚みが３μｍ以下の積層型電子部品を得ようとしても、ショート不良を無くし、高温負荷寿命を得る等、信頼性を確保することは困難である。
本発明は、上記実状に鑑みてなされたものであり、容易に製造可能な、スラリー、グリーンシート及び積層型電子部品ならびにこれらの製造方法を提供することを目的とする。
また、本発明は、品質、信頼性等が低下することなく、薄層化された積層型電子部品を製造可能な、スラリー、グリーンシート及び積層型電子部品ならびにこれらの製造方法を提供することを目的とする。
さらに、本発明は、添加剤の分散性を向上させることができるスラリー及びスラリーの製造方法を提供することを目的とする。
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a slurry, a green sheet, a multilayer electronic component, and a manufacturing method thereof that can be easily manufactured.
In addition, the present invention provides a slurry, a green sheet, a multilayer electronic component, and a method for manufacturing the same, which can manufacture a laminated electronic component having a reduced thickness without degrading quality, reliability, and the like. Objective.
Furthermore, this invention aims at providing the manufacturing method of the slurry which can improve the dispersibility of an additive, and a slurry.
上記目的を達成するため、この発明の第１の観点にかかるスラリーの製造方法は、
溶剤に誘電体粉末と添加剤とが分散されたスラリーの製造方法であって、
前記添加剤を作製する添加剤作製工程と、
前記添加剤作製工程で作製された添加剤を粉砕する粉砕工程と、
少なくとも、前記粉砕工程で粉砕された添加剤と、前記誘電体粉末と、前記溶剤とを混合、粉砕してスラリーを作製するスラリー作製工程と、
を備え、
前記粉砕工程では、前記スラリー作製工程で混合される溶剤の少なくとも１つの溶剤を用いて湿式粉砕を行う、ことを特徴とする。
In order to achieve the above object, a method for producing a slurry according to the first aspect of the present invention comprises:
A method for producing a slurry in which a dielectric powder and an additive are dispersed in a solvent,
An additive preparation step of preparing the additive;
A pulverization step of pulverizing the additive prepared in the additive preparation step;
At least an additive pulverized in the pulverization step, the dielectric powder, and the solvent are mixed and pulverized to prepare a slurry, and a slurry preparation step,
With
In the pulverization step, wet pulverization is performed using at least one of the solvents mixed in the slurry preparation step.
この構成によれば、スラリー作製工程で混合される溶剤の少なくとも１つの溶剤を用いて湿式粉砕が行われるので、粉砕した添加剤を乾燥する必要が無くなり、工程の簡略化が図れる。また乾燥しないため、乾燥による凝集が抑えることができ、粗粒子の発生が無くなり、粗粒子混入の不具合がなくなる。 According to this configuration, wet pulverization is performed using at least one of the solvents mixed in the slurry preparation process, so that it is not necessary to dry the pulverized additive, and the process can be simplified. Moreover, since it does not dry, aggregation by drying can be suppressed, generation | occurrence | production of a coarse particle is eliminated, and the malfunction of coarse particle mixing is eliminated.
前記粉砕工程で湿式粉砕された添加剤にバインダーを添加するバインダー添加工程をさらに備えることが好ましい。湿式粉砕された添加剤にバインダーを添加することにより、粘度がある程度高くなり、添加剤の再凝集や分離が抑えられる。また、バインダーの分散効果により、添加剤の再凝集が抑えられる。 It is preferable to further include a binder addition step of adding a binder to the additive wet-pulverized in the pulverization step. By adding a binder to the wet pulverized additive, the viscosity is increased to some extent, and re-aggregation and separation of the additive are suppressed. Further, the re-aggregation of the additive is suppressed by the binder dispersing effect.
前記バインダー添加工程では、バインダー添加後の粘度が４０ｍＰａ・ｓ〜５００ｍＰａ・ｓとなるように、バインダーを添加することが好ましい。 In the binder addition step, it is preferable to add a binder so that the viscosity after addition of the binder is 40 mPa · s to 500 mPa · s.
前記粉砕工程では、添加剤の平均粒径が０．４μｍ以下になるように、添加剤を粉砕することが好ましい。この場合、添加剤の分散性が向上し、製品の信頼性を上げることができる。 In the pulverization step, the additive is preferably pulverized so that the average particle size of the additive is 0.4 μm or less. In this case, the dispersibility of the additive is improved and the reliability of the product can be increased.
前記粉砕工程では、添加剤の平均粒径が前記誘電体粉末の平均粒径の６２％以下の粒径になるように、添加剤を粉砕することが好ましい。 In the pulverization step, the additive is preferably pulverized so that the average particle diameter of the additive is 62% or less of the average particle diameter of the dielectric powder.
この発明の第２の観点にかかるスラリーは、第１の観点にかかるスラリーの製造方法により製造されることを特徴とする。 The slurry according to the second aspect of the present invention is manufactured by the slurry manufacturing method according to the first aspect.
この発明の第３の観点にかかるグリーンシートの製造方法は、第１の観点にかかるスラリーの製造方法により製造されたスラリーを用いてグリーンシートを形成する工程を有する、ことを特徴とする。 The green sheet manufacturing method according to the third aspect of the present invention includes a step of forming a green sheet using the slurry manufactured by the slurry manufacturing method according to the first aspect.
この発明の第４の観点にかかるグリーンシートは、第３の観点にかかるグリーンシートの製造方法により製造される、ことを特徴とする。 A green sheet according to a fourth aspect of the present invention is manufactured by the method for manufacturing a green sheet according to the third aspect.
この発明の第５の観点にかかる積層型電子部品の製造方法は、第１の観点にかかるスラリーの製造方法により製造されたスラリーを用いて形成したグリーンシートを形成する工程と、
形成されたグリーンシートを積層する工程を備える、ことを特徴とする。
A method for manufacturing a multilayer electronic component according to a fifth aspect of the present invention includes a step of forming a green sheet formed using the slurry manufactured by the slurry manufacturing method according to the first aspect;
A step of laminating the formed green sheets.
この発明の第６の観点にかかる積層型電子部品は、第５の観点にかかる積層型電子部品の製造方法により製造される、ことを特徴とする。 A multilayer electronic component according to a sixth aspect of the present invention is manufactured by the method for manufacturing a multilayer electronic component according to the fifth aspect.
この発明によれば、容易に製造可能な、スラリー、グリーンシート及び積層型電子部品ならびにこれらの製造方法を提供することができる。 According to the present invention, it is possible to provide a slurry, a green sheet, a multilayer electronic component, and a manufacturing method thereof that can be easily manufactured.
以下、本発明の実施の形態に係るスラリー、グリーンシート及び積層型電子部品ならびにこれらの製造方法について、詳細に説明する。なお、以下では、積層セラミックコンデンサを製造する場合を例として説明する。 Hereinafter, the slurry, the green sheet, the multilayer electronic component, and the manufacturing method thereof according to the embodiment of the present invention will be described in detail. In the following, a case where a multilayer ceramic capacitor is manufactured will be described as an example.
本実施の形態に係るスラリーは、誘電体粉末と、有機バインダーと、添加剤と、溶剤と、その他必要な添加剤とを含んで構成される。 The slurry according to the present embodiment includes a dielectric powder, an organic binder, an additive, a solvent, and other necessary additives.
誘電体粉末としては、セラミック粉末が使用可能である。セラミック粉末は、一般的に積層型電子部品の製造に使用される材料粉末であればよく、チタン酸バリウム等のチタン酸化物の他に、アルミニウム、バリウム、鉛、ジルコニウム、ケイ素、イットリウム等の酸化物あるいはこれらの混合物が使用可能である。誘電体粉末には、所定の粒度のものが用いられる。 Ceramic powder can be used as the dielectric powder. The ceramic powder may be any material powder that is generally used for the production of multilayer electronic components. In addition to titanium oxide such as barium titanate, oxidation of aluminum, barium, lead, zirconium, silicon, yttrium, etc. Or mixtures thereof can be used. A dielectric powder having a predetermined particle size is used.
有機バインダーとしては、ブチラール系、アクリル系、オレフィン系等の樹脂を用いることができる。 As the organic binder, a butyral resin, an acrylic resin, an olefin resin, or the like can be used.
添加剤としては、バリウム、カルシウム、または珪素等を含む金属酸化物を所定の比率にて混合・分散し、仮焼きしたものを用いることが可能である。ここで、添加剤は、その平均粒径を、一定粒径、例えば、０．４μｍ以下にして分散性を向上させることが好ましい。また、添加剤は、誘電体粉末の平均粒径の６２％以下の粒径にして分散性を向上させることが好ましい。 As the additive, a metal oxide containing barium, calcium, silicon or the like mixed and dispersed at a predetermined ratio and calcined can be used. Here, it is preferable to improve the dispersibility by setting the average particle size of the additive to a constant particle size, for example, 0.4 μm or less. Further, it is preferable that the additive has a particle size of 62% or less of the average particle size of the dielectric powder to improve the dispersibility.
溶剤は、トルエン等の芳香族炭化水素、メチルエチルケトン等のケトン、エチルアルコール等のアルコールといった一般的な有機溶剤が使用可能である。 As the solvent, general organic solvents such as aromatic hydrocarbons such as toluene, ketones such as methyl ethyl ketone, and alcohols such as ethyl alcohol can be used.
以下、上記した本実施の形態に係るスラリー、グリーンシート及び積層型電子部品の製造方法について説明する。なお、本例では、積層セラミックコンデンサを製造する場合について説明する。図１に積層セラミックコンデンサの製造工程を示す。 Hereinafter, the manufacturing method of the slurry, the green sheet, and the multilayer electronic component according to the above-described embodiment will be described. In this example, a case where a multilayer ceramic capacitor is manufactured will be described. FIG. 1 shows a manufacturing process of a multilayer ceramic capacitor.
まず、スラリーの添加剤となるバリウム、カルシウム、または珪素等を含む金属酸化物を所定の比率に調合する（ステップＳ１）。次に、ボールミル等の分散機で混合・粉砕を行った後（ステップＳ２）、所定温度で所定時間乾燥（ステップＳ３）、仮焼き（ステップＳ４）を行い、添加剤を完成させる（ステップＳ５）。 First, a metal oxide containing barium, calcium, silicon or the like serving as an additive for the slurry is prepared in a predetermined ratio (step S1). Next, after mixing and pulverizing with a disperser such as a ball mill (step S2), drying is performed at a predetermined temperature for a predetermined time (step S3) and calcining (step S4) to complete the additive (step S5). .
続いて、完成した添加剤に、後述するステップＳ８で用いる溶剤の少なくとも１つを含む有機溶剤を加えて湿式粉砕を行い（ステップＳ６）、所定のバインダーを投入（混合）する（ステップＳ７）。 Subsequently, an organic solvent containing at least one of the solvents used in step S8, which will be described later, is added to the completed additive to perform wet grinding (step S6), and a predetermined binder is charged (mixed) (step S7).
ここで、粉砕後の添加剤は、その平均粒径を０．４μｍ以下にすることが好ましい。また、添加剤は、誘電体粉末の平均粒径の６２％以下の粒径にすることが好ましい。平均粒径が０．４μｍ以下、誘電体粉末の平均粒径の６２％以下の粒径であると、添加剤の分散性が向上し、製造される製品の信頼性を上げることができるためである。添加材の粒度は、混合・粉砕時間、分散機に用いるメディアの粒径、量などで変化させる。 Here, the pulverized additive preferably has an average particle size of 0.4 μm or less. Further, the additive preferably has a particle size of 62% or less of the average particle size of the dielectric powder. When the average particle size is 0.4 μm or less and the particle size is 62% or less of the average particle size of the dielectric powder, the dispersibility of the additive is improved and the reliability of the manufactured product can be increased. is there. The particle size of the additive is changed depending on the mixing and grinding time, the particle size and amount of the media used in the disperser, and the like.
また、ステップＳ６の湿式粉砕（仮焼き後の粉砕）を水で行わず、後述するステップＳ８で用いる溶剤の少なくとも１つを含む溶剤を用いているので、その後に乾燥（従来のステップＳ５７）、予備粉砕（従来のステップＳ５８）を行うことなく、そのまま誘電体粉末との混合・粉砕（ステップＳ８）を行うことができる。このため、製造工程の簡略化が図れる。また、乾燥工程をなくすことができるため、乾燥後の凝集が押さえられ、粗粒子の発生が無くなり、粗粒子混入の不具合がなくなる。 Also, since the wet pulverization (calcination after calcination) in step S6 is not performed with water, a solvent containing at least one of the solvents used in step S8 described later is used, and thereafter drying (conventional step S57), Without preliminary pulverization (conventional step S58), mixing and pulverization (step S8) with the dielectric powder can be performed as it is. For this reason, the manufacturing process can be simplified. Further, since the drying process can be eliminated, aggregation after drying is suppressed, the generation of coarse particles is eliminated, and the problem of mixing coarse particles is eliminated.
また、所定のバインダーを混合しているので粘度が上がり、細粒化した添加剤の再凝集や分離を防ぐことができる。バインダー添加後の粘度は、例えば、４０ｍＰａ・ｓ〜５００ｍＰａ・ｓであることが好ましい。さらに、バインダーの分散効果により細粒化した添加剤の再凝集を防ぐことができる。このため、添加剤の分散性を向上させることができる。 Moreover, since the predetermined binder is mixed, the viscosity is increased, and re-aggregation and separation of the finely divided additive can be prevented. The viscosity after adding the binder is preferably 40 mPa · s to 500 mPa · s, for example. Furthermore, re-aggregation of the additive finely divided by the binder dispersing effect can be prevented. For this reason, the dispersibility of an additive can be improved.
次に、チタン酸バリウム等の誘電体粉末、所定の有機溶剤、所定のバインダー、その他添加剤を加えて、ボールミル等の分散機で添加剤と誘電体粉末との混合・粉砕を行う（ステップＳ８）。これにより、スラリーが完成する（ステップＳ９）。なお、得られたスラリーを攪拌することで沈降分離を防止でき、長期的保存においても安定した形態をとることができる。 Next, a dielectric powder such as barium titanate, a predetermined organic solvent, a predetermined binder, and other additives are added, and the additive and the dielectric powder are mixed and pulverized by a dispersing machine such as a ball mill (step S8). ). Thereby, a slurry is completed (step S9). In addition, by stirring the obtained slurry, sedimentation separation can be prevented, and a stable form can be obtained even in long-term storage.
続いて、このスラリーを、シリコーン等の剥離剤が塗布されたポリエチレンテレフタレート（ＰＥＴ）フィルム等の支持体上に、例えば、ドクターブレード法により塗布し、その後、例えば、７０℃で乾燥させて溶媒をとばし、セラミックグリーンシートを形成する（ステップＳ１０）。 Subsequently, the slurry is applied onto a support such as a polyethylene terephthalate (PET) film coated with a release agent such as silicone by, for example, a doctor blade method, and then dried at, for example, 70 ° C. to remove the solvent. By skipping, a ceramic green sheet is formed (step S10).
次に、このセラミックグリーンシートの上に、パラジウム、銀−パラジウム、ニッケル等の内部電極となる金属と有機溶剤等とを含む電極ペーストを用い、所定の電極パターンを形成する。その後、印刷されたセラミックグリーンシートを支持体より剥離する。次いで、このように形成された複数枚のセラミックグリーンシートを積層し、厚み方向にプレスして圧着する（ステップＳ１１）。 Next, a predetermined electrode pattern is formed on the ceramic green sheet using an electrode paste containing a metal that becomes an internal electrode such as palladium, silver-palladium, or nickel and an organic solvent. Thereafter, the printed ceramic green sheet is peeled off from the support. Next, a plurality of ceramic green sheets formed in this way are stacked, pressed in the thickness direction, and pressure-bonded (step S11).
続いて、圧着された積層体を、個々のセラミックコンデンサを得るための積層体が得られるように切断し、有機バインダー、可塑剤等を熱処理等で除去した後、焼成して焼結体とする。最後に、内部電極と導通する外部電極を焼き付けることにより、積層セラミックコンデンサが得られる（ステップＳ１２）。 Subsequently, the pressure-bonded laminated body is cut so as to obtain a laminated body for obtaining individual ceramic capacitors, and the organic binder, plasticizer, and the like are removed by heat treatment and then fired to obtain a sintered body. . Finally, a multilayer ceramic capacitor is obtained by baking an external electrode that is electrically connected to the internal electrode (step S12).
本実施の形態によれば、添加剤の製造時において、仮焼き後の湿式粉砕に水を用いずに、誘電体粉末との調合時に使用される有機溶剤を用いて湿式粉砕を行っているので、その後の乾燥工程を行わずに、そのまま誘電体粉末との調合を行うことができる。このため、製造工程の簡略化を図ることができる。また、乾燥工程をなくすことができるため、乾燥後の凝集が押さえられ、粗粒子の発生が無くなり、粗粒子混入の不具合がなくなる。 According to the present embodiment, when the additive is manufactured, the wet pulverization is performed using the organic solvent used in the preparation with the dielectric powder without using water for the wet pulverization after the calcining. And without performing the subsequent drying process, it can mix | blend with dielectric material powder as it is. For this reason, the manufacturing process can be simplified. Further, since the drying process can be eliminated, aggregation after drying is suppressed, the generation of coarse particles is eliminated, and the problem of mixing coarse particles is eliminated.
また、本実施の形態によれば、仮焼き後の湿式粉砕の後に、所定のバインダーを混合しているので、細粒化した添加剤の再凝集や分離を防ぐことができる。このため、添加剤の分散性を向上させることができる。 Moreover, according to this Embodiment, since the predetermined binder is mixed after the wet pulverization after calcination, re-aggregation and separation of the finely divided additive can be prevented. For this reason, the dispersibility of an additive can be improved.
本発明は、上記実施の形態に限られず、種々の変形、応用が可能である。 The present invention is not limited to the above embodiment, and various modifications and applications are possible.
上記実施の形態では、ステップＳ７でバインダを投入した場合を例として説明したが、例えば、バインダを投入せずに、誘電体粉末との混合・粉砕を行ってもよい。この場合にも、製造工程の簡略化を図ることができるとともに、粗粒子混入の不具合がなくなる。 In the above-described embodiment, the case where the binder is added in step S7 has been described as an example. However, for example, mixing and pulverization with the dielectric powder may be performed without adding the binder. In this case as well, the manufacturing process can be simplified and the problem of mixing coarse particles is eliminated.
上記実施の形態では、平均粒径が０．６５μｍの誘電体粉末を用いた場合を例として説明したが、例えば、平均粒径が２μｍの誘電体粉末を用いてもよい。この場合にも、仮焼き後の湿式粉砕に誘電体粉末との調合時に使用される有機溶剤を用いて湿式粉砕を行うことにより、製造工程の簡略化を図ることができ、粗粒子の発生が無くなり、粗粒子混入の不具合がなくなる。また、誘電体粉末の平均粒径が大きくなった場合にも、添加剤の粒径を誘電体粉末の平均粒径の６２％以下の粒径にすることが好ましい。この場合、添加剤の分散性がさらに向上し、製造される製品の信頼性を上げることができる。 In the above embodiment, the case where the dielectric powder having an average particle diameter of 0.65 μm is used as an example. However, for example, a dielectric powder having an average particle diameter of 2 μm may be used. Also in this case, by performing wet pulverization using an organic solvent used in the preparation with the dielectric powder for wet pulverization after calcination, the manufacturing process can be simplified, and generation of coarse particles can be achieved. This eliminates the problem of coarse particle contamination. Even when the average particle size of the dielectric powder is increased, it is preferable to set the particle size of the additive to 62% or less of the average particle size of the dielectric powder. In this case, the dispersibility of the additive can be further improved, and the reliability of the manufactured product can be increased.
上記実施の形態では、分散機としてボールミルを用いた場合を例として説明したが、例えば、メディアミルを用いてもよい。また、高圧型分散機を併用してもよい。 In the above embodiment, the case where a ball mill is used as the disperser has been described as an example. However, for example, a media mill may be used. Further, a high-pressure disperser may be used in combination.
上記実施の形態では、積層セラミックコンデンサを例として説明した。しかし、勿論、上記例に限らず、本発明は、積層インダクタ、積層アクチュエータ、積層ＬＣフィルタ等あるいはこれらの複合電子部品にも適用可能である。 In the above embodiment, a multilayer ceramic capacitor has been described as an example. However, of course, the present invention is not limited to the above example, and the present invention can also be applied to multilayer inductors, multilayer actuators, multilayer LC filters, and the like, or composite electronic components thereof.
以下、本実施の形態の具体的実施例を挙げ、本発明をさらに詳細に説明する。本実施例のスラリー、このスラリーを用いたセラミックグリーンシート、積層セラミックコンデンサを作製し、その特性について調べた。 Hereinafter, the present invention will be described in more detail with reference to specific examples of the present embodiment. A slurry of this example, a ceramic green sheet using this slurry, and a multilayer ceramic capacitor were produced, and their characteristics were examined.
本実施例では、仮焼き後の添加剤に有機溶剤等を加えて湿式粉砕を行い、バインダーを混合した後、誘電体粉末、有機溶剤、バインダー、その他添加剤を加えて、ボールミル等の分散機で混合・粉砕を行い、スラリーを作製した。 In this example, an organic solvent or the like is added to the additive after calcining and wet pulverization is performed. After mixing the binder, a dielectric powder, an organic solvent, a binder, and other additives are added, and a dispersing machine such as a ball mill. The mixture was crushed and ground to prepare a slurry.
誘電体粉末と混合する前の添加剤粉砕時の組成は、表１に示すように、添加剤としてのBa,Ca,Mg,Y,Si-酸化物が３１．７重量％、有機溶剤としてのエタノールが６６．７重量％、バインダーとしてのブチラール樹脂が１．０重量％、分散剤・その他としての可塑剤（ＤＯＰ：ジオクチルフタレート）が０．６重量％となるように作製した。 As shown in Table 1, the composition at the time of pulverizing the additive before mixing with the dielectric powder was 31.7% by weight of Ba, Ca, Mg, Y, Si-oxide as an additive, and as an organic solvent. It was prepared such that ethanol was 66.7% by weight, butyral resin as a binder was 1.0% by weight, and plasticizer (DOP: dioctyl phthalate) as a dispersant and others was 0.6% by weight.
実施例１では、添加剤粉砕時の添加剤の平均粒径は、０．５１μｍであり、粘度は３０（ｍＰａ・ｓ）であった。また、実施例２〜５では、混合・粉砕時間、分散機に用いるメディアの粒径、量などで変化させ、添加剤の平均粒径、粘度を実施例１から変化させた。 In Example 1, the average particle size of the additive at the time of pulverizing the additive was 0.51 μm, and the viscosity was 30 (mPa · s). In Examples 2 to 5, the average particle size and viscosity of the additive were changed from those in Example 1 by changing the mixing and grinding time, the particle size and amount of the media used in the disperser, and the like.
そして、誘電体粉末としてのチタン酸バリウム１００重量部に対して、添加剤が６．８重量部、バインダーが６．２重量部、有機溶剤・分散剤を１１５．３重量部となるように秤量し、ボールミル等の分散機で混合、分散することによりスラリーを作製した。なお、有機溶剤、バインダー等は、通常入れる量より添加剤のスラリーから入る量を引いて秤量した。また、誘電体粉末は、その平均粒径が０．６５μｍのものを用いた。 Then, 100 parts by weight of barium titanate as the dielectric powder is weighed so that the additive is 6.8 parts by weight, the binder is 6.2 parts by weight, and the organic solvent / dispersant is 115.3 parts by weight. Then, a slurry was prepared by mixing and dispersing with a dispersing machine such as a ball mill. In addition, the organic solvent, the binder, and the like were weighed by subtracting the amount added from the additive slurry from the amount normally added. The dielectric powder having an average particle size of 0.65 μm was used.
比較例では、仮焼き後の添加剤に水等を加えて湿式粉砕を行い、乾燥、予備粉砕を行った後、実施例と同様に、誘電体粉末、有機溶剤、バインダー、その他添加剤を加えて、ボールミル等の分散機で混合・粉砕を行い、スラリーを作製した。 In the comparative example, water was added to the additive after calcining and wet pulverization was performed, followed by drying and preliminary pulverization. Then, similar to the examples, dielectric powder, organic solvent, binder, and other additives were added. Then, mixing and pulverization were performed with a dispersing machine such as a ball mill to prepare a slurry.
なお、実施例５、比較例３では、添加剤粉砕後の添加剤スラリーに凝集（凝化）がおきているが、誘電体粉末との分散時には安定化しており、スラリー製造においては問題は生じなかった。これは、添加剤スラリーで凝集がおきても基本的に細かくなっており、誘電体スラリー分散時には再分散されるためである。なお、凝集の度合いは、実施例５では僅かであり、比較例３では多かった。 In Example 5 and Comparative Example 3, agglomeration (coagulation) occurs in the additive slurry after pulverization of the additive, but it is stabilized at the time of dispersion with the dielectric powder, and there is a problem in slurry production. There wasn't. This is because even if aggregation occurs in the additive slurry, it is basically fine and is redispersed when the dielectric slurry is dispersed. The degree of aggregation was slight in Example 5 and large in Comparative Example 3.
このように作製した実施例１〜５、比較例１〜３のスラリーをＰＥＴフィルムにドクターブレード法により塗布し、電極をスクリーン印刷し、積層機でＰＥＴフィルムから剥離、積層し、プレスで熱圧着し、所定の形状に切断し、セラミックグリーンチップを作成した。なお、層数は２５０層であり、層間は焼き上げ４μｍである。 The slurry of Examples 1 to 5 and Comparative Examples 1 to 3 thus prepared was applied to a PET film by a doctor blade method, electrodes were screen printed, peeled from the PET film with a laminator, laminated, and thermocompression bonded with a press. Then, it was cut into a predetermined shape to produce a ceramic green chip. The number of layers is 250, and the layers are baked 4 μm.
作製した実施例および比較例にかかるセラミックグリーンチップの諸特性は、信頼性、ショート不良、および耐圧不良について調べた。信頼性（加速試験）は、電圧を定格の３倍、温度２００℃とし、実施例１の故障時間の平均値を１としたときの、それぞれの故障時間の平均値の比で示した。また、ショート不良および耐圧不良は、コンデンサチップについて一般的な評価方法でその不良率を調べた。表１に実施例及び比較例にかかる信頼性、ショート不良及び耐圧不良の結果を示す。また、図２に実施例１〜５にかかる信頼性、ショート不良及び耐圧不良の結果を示す。 Various characteristics of the produced ceramic green chips according to the example and the comparative example were examined with respect to reliability, short circuit failure, and breakdown voltage failure. The reliability (acceleration test) is represented by the ratio of the average value of each failure time when the voltage is 3 times the rating, the temperature is 200 ° C., and the average value of the failure time in Example 1 is 1. Moreover, the defect rate was investigated by the general evaluation method about the capacitor | condenser chip about the short circuit defect and the pressure | voltage resistant defect. Table 1 shows the results of reliability, short-circuit failure, and breakdown voltage failure according to Examples and Comparative Examples. FIG. 2 shows the results of reliability, short-circuit failure, and breakdown voltage failure according to Examples 1-5.
添加剤の平均粒径の等しい実施例１と比較例１、実施例３と比較例２、実施例５と比較例３を比較すると、表１に示すように、仮焼き後の添加剤に有機溶剤等を加えた本発明の製造方法で製造したスラリーを用いることにより、ショート不良及び耐圧不良となる割合を低下させることができるとともに、信頼性を向上させることができることがわかる。これは、添加剤仮焼き後の乾燥工程をなくすことができるため、乾燥後の凝集が押さえられ、粗粒子の発生が無くなり、粗粒子混入の不具合がなくなるためであると考えられる。また、本発明の製造方法で製造したスラリーを用いることにより、乾燥工程をなくすことができるため、製造工程の簡略化を図ることができる。 When Example 1 and Comparative Example 1 having the same average particle diameter of the additive were compared, Example 3 and Comparative Example 2, and Example 5 and Comparative Example 3 were compared, as shown in Table 1, the additive after calcination was organic. It can be seen that by using the slurry produced by the production method of the present invention to which a solvent or the like is added, the ratio of short circuit failure and breakdown voltage failure can be reduced and the reliability can be improved. This is considered to be because the drying step after the additive calcination can be eliminated, so that aggregation after drying is suppressed, the generation of coarse particles is eliminated, and the problem of mixing coarse particles is eliminated. Moreover, since the drying process can be eliminated by using the slurry produced by the production method of the present invention, the production process can be simplified.
添加剤の平均粒径の異なる実施例１〜５を比較すると、図２に示すように、添加剤の平均粒径を０．４μｍ以下（誘電体粉末の平均粒径の６２％以下の粒径）とすることにより、ショート不良及び耐圧不良となる割合をさらに低下させることができるとともに、信頼性をさらに向上させることができることがわかる。これは、添加剤の平均粒径を０．４μｍ以下のように小さくすることにより、添加剤の分散性が向上し、製造される製品の信頼性を上げることができるためである。このため、添加剤は、その平均粒径を０．４μｍ以下にすることが好ましい。 When Examples 1 to 5 having different average particle diameters of the additives are compared, as shown in FIG. 2, the average particle diameter of the additives is 0.4 μm or less (a particle diameter of 62% or less of the average particle diameter of the dielectric powder). ), The ratio of short circuit failure and breakdown voltage failure can be further reduced, and the reliability can be further improved. This is because by reducing the average particle size of the additive to 0.4 μm or less, the dispersibility of the additive is improved and the reliability of the manufactured product can be increased. For this reason, the additive preferably has an average particle size of 0.4 μm or less.
Claims (10)
前記添加剤を作製する添加剤作製工程と、
前記添加剤作製工程で作製された添加剤を粉砕する粉砕工程と、
少なくとも、前記粉砕工程で粉砕された添加剤と、前記誘電体粉末と、前記溶剤とを混合、粉砕してスラリーを作製するスラリー作製工程と、
を備え、
前記粉砕工程では、前記スラリー作製工程で混合される溶剤の少なくとも１つの溶剤を用いて湿式粉砕を行う、ことを特徴とするスラリーの製造方法。 A method for producing a slurry in which a dielectric powder and an additive are dispersed in a solvent,
An additive preparation step of preparing the additive;
A pulverization step of pulverizing the additive prepared in the additive preparation step;
At least an additive pulverized in the pulverization step, the dielectric powder, and the solvent are mixed and pulverized to prepare a slurry, and a slurry preparation step,
With
In the pulverization step, wet pulverization is performed using at least one of the solvents mixed in the slurry preparation step.
形成されたグリーンシートを積層する工程を備える、ことを特徴とする積層型電子部品の製造方法。 Forming a green sheet formed using the slurry manufactured by the slurry manufacturing method according to any one of claims 1 to 5,
A method for producing a multilayer electronic component, comprising: a step of laminating formed green sheets.
A multilayer electronic component manufactured by the multilayer electronic component manufacturing method according to claim 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003341306A JP4506138B2 (en) | 2003-09-30 | 2003-09-30 | Method for producing slurry, method for producing green sheet, and method for producing multilayer electronic component |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003341306A JP4506138B2 (en) | 2003-09-30 | 2003-09-30 | Method for producing slurry, method for producing green sheet, and method for producing multilayer electronic component |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2005104782A true JP2005104782A (en) | 2005-04-21 |
| JP4506138B2 JP4506138B2 (en) | 2010-07-21 |
Family
ID=34535945
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2003341306A Expired - Lifetime JP4506138B2 (en) | 2003-09-30 | 2003-09-30 | Method for producing slurry, method for producing green sheet, and method for producing multilayer electronic component |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4506138B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007137693A (en) * | 2005-11-15 | 2007-06-07 | Tdk Corp | Method for producing ceramic slurry |
| KR100762797B1 (en) * | 2005-12-28 | 2007-10-02 | 한국전기연구원 | Electrode For Energy Storage Device And Manufacturing Method thereof |
| JP2008251699A (en) * | 2007-03-29 | 2008-10-16 | Tdk Corp | Manufacturing method of multilayer electronic part |
| JP2009155143A (en) * | 2007-12-25 | 2009-07-16 | Samsung Electro Mech Co Ltd | Method for producing dielectric ceramic material |
| JP2009155142A (en) * | 2007-12-25 | 2009-07-16 | Samsung Electro Mech Co Ltd | Method for producing ceramic slurry |
| KR20200133410A (en) | 2019-05-20 | 2020-11-30 | 홍익대학교 산학협력단 | Barium titanate mixed powder and manufacturing method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10255549A (en) * | 1997-03-05 | 1998-09-25 | Tdk Corp | Dielectric ceramic material, its manufacture, and laminated ceramic capacitor |
| JPH10270284A (en) * | 1997-03-24 | 1998-10-09 | Tdk Corp | Manufacture of dielectric ceramic material |
| JP2000203941A (en) * | 1999-01-11 | 2000-07-25 | Tdk Corp | Production of ceramic paste |
| JP2001172076A (en) * | 1999-10-05 | 2001-06-26 | Tdk Corp | Method for producing dielectric ceramic composition |
| JP2003192449A (en) * | 2001-12-27 | 2003-07-09 | Tdk Corp | Water-based coating composition for ceramic green sheet, method for manufacturing ceramic green sheet and method for manufacturing ceramic electronic parts |
-
2003
- 2003-09-30 JP JP2003341306A patent/JP4506138B2/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10255549A (en) * | 1997-03-05 | 1998-09-25 | Tdk Corp | Dielectric ceramic material, its manufacture, and laminated ceramic capacitor |
| JPH10270284A (en) * | 1997-03-24 | 1998-10-09 | Tdk Corp | Manufacture of dielectric ceramic material |
| JP2000203941A (en) * | 1999-01-11 | 2000-07-25 | Tdk Corp | Production of ceramic paste |
| JP2001172076A (en) * | 1999-10-05 | 2001-06-26 | Tdk Corp | Method for producing dielectric ceramic composition |
| JP2003192449A (en) * | 2001-12-27 | 2003-07-09 | Tdk Corp | Water-based coating composition for ceramic green sheet, method for manufacturing ceramic green sheet and method for manufacturing ceramic electronic parts |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007137693A (en) * | 2005-11-15 | 2007-06-07 | Tdk Corp | Method for producing ceramic slurry |
| JP4687412B2 (en) * | 2005-11-15 | 2011-05-25 | Ｔｄｋ株式会社 | Method for producing ceramic slurry |
| KR100762797B1 (en) * | 2005-12-28 | 2007-10-02 | 한국전기연구원 | Electrode For Energy Storage Device And Manufacturing Method thereof |
| JP2008251699A (en) * | 2007-03-29 | 2008-10-16 | Tdk Corp | Manufacturing method of multilayer electronic part |
| JP2009155143A (en) * | 2007-12-25 | 2009-07-16 | Samsung Electro Mech Co Ltd | Method for producing dielectric ceramic material |
| JP2009155142A (en) * | 2007-12-25 | 2009-07-16 | Samsung Electro Mech Co Ltd | Method for producing ceramic slurry |
| KR20200133410A (en) | 2019-05-20 | 2020-11-30 | 홍익대학교 산학협력단 | Barium titanate mixed powder and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4506138B2 (en) | 2010-07-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP3675264B2 (en) | Method for manufacturing ceramic slurry, ceramic green sheet and multilayer ceramic electronic component | |
| JP2013098528A (en) | Multilayer ceramic capacitor | |
| JP2015156470A (en) | Laminated ceramic electronic component | |
| JP2001114569A (en) | Ceramic slurry composition, ceramic green sheet and production of multilayer ceramic electronic part | |
| JP2013089946A (en) | Multilayer ceramic electronic part | |
| JP6329236B2 (en) | Dielectric material for multilayer ceramic capacitor and multilayer ceramic capacitor | |
| JP3783678B2 (en) | Method for producing raw material powder for dielectric ceramic, dielectric ceramic and multilayer ceramic capacitor | |
| JP4506138B2 (en) | Method for producing slurry, method for producing green sheet, and method for producing multilayer electronic component | |
| US20120048452A1 (en) | Method of manufacturing ceramic paste for multilayer ceramic electronic component and method of manufacturing multilayer ceramic electronic component having the same | |
| KR20110074486A (en) | Method for manufacturing dielectric ceramic material | |
| JP2004345873A (en) | Paste, production method therefor, multilayer ceramic electronic part, and production method therefor | |
| JP2001039773A (en) | Production of ceramic slurry, ceramic green sheet and laminated ceramic electronic parts | |
| JP2010195639A (en) | Method of preparing ceramic slurry, method of manufacturing ceramic powder, ceramic powder, and method of forming ceramic green sheet | |
| JP4601438B2 (en) | Green sheet manufacturing method | |
| JP4930149B2 (en) | Manufacturing method of multilayer electronic component | |
| TW202119441A (en) | Electrically conductive paste composition for laminated ceramic capacitor internal electrode, method for manufacturing said electrically conductive paste composition for laminated ceramic capacitor internal electrode, and electrically conductive paste | |
| JP6809280B2 (en) | Method of manufacturing conductive paste | |
| JP5184333B2 (en) | Method for manufacturing dielectric ceramic material | |
| JP2002121079A (en) | Method of producing superfine particulate barium titanate dielectric ceramic material | |
| JP3538706B2 (en) | Method for producing ceramic slurry composition and method for producing ceramic green sheet | |
| JP5459951B2 (en) | Method for producing ceramic slurry | |
| JP6844299B2 (en) | Method of manufacturing conductive paste | |
| KR100951319B1 (en) | Manufacturing method of dielectric ceramic material, green sheet, sintered body and multi layered ceramic condenser using dielectric material manufactured thereby | |
| JP2009143734A (en) | Method for manufacturing dielectric material | |
| JP2008239420A (en) | Method for manufacturing ceramic green sheet, ceramic green sheet, and ceramic capacitor using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20060510 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20081215 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20081224 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20090216 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20090908 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20091104 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20100406 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20100419 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130514 Year of fee payment: 3 |
|
| R150 | Certificate of patent or registration of utility model |
Ref document number: 4506138 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140514 Year of fee payment: 4 |
|
| EXPY | Cancellation because of completion of term |