CN101752082A - Method for preparing Ag inner electrode multilayer ceramic capacitors - Google Patents

Method for preparing Ag inner electrode multilayer ceramic capacitors Download PDF

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Publication number
CN101752082A
CN101752082A CN200810239688A CN200810239688A CN101752082A CN 101752082 A CN101752082 A CN 101752082A CN 200810239688 A CN200810239688 A CN 200810239688A CN 200810239688 A CN200810239688 A CN 200810239688A CN 101752082 A CN101752082 A CN 101752082A
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multilayer ceramic
inner electrode
glass
temperature
auxiliary material
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吉岸
袁纪烈
陈月光
王士娇
张力
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Shandong And Electronics Co Ltd Of Square Shandong Tip
Tsinghua Tongfang Co Ltd
Tongfang Co Ltd
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Shandong And Electronics Co Ltd Of Square Shandong Tip
Tongfang Co Ltd
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Abstract

A method for preparing Ag inner electrode multilayer ceramic capacitors relates to the technical field of ceramic materials. The method of the invention comprises the steps that: (1)aBao-bLn2O3-cBi2O3-dTiO2 serving as the mother material, eBi2O3-fB2O3-gZnO-hSiO2 glass serving and jBaO-kLi2O-lCaO-mSrO-nSiO2 glass which serve as the auxiliary materials are mixed with each other to form the mixture; (2) the mixture ball milled is dried; (3) the mixture is mixed with organic solvent and the obtained mixture is ball milled to overlap the dielectric layer with the Ag inner electrode to form the unfired body of the multilayer ceramic capacitor; (4) the temperature of the unfired body is maintained at a temperature of 300 DEG C; (5) the unfired body is sintered in the air atmosphere; (6) the unfired body is cooled down to the room temperature; (7) the temperature of the Ag inner electrode used as the unfired body of a terminal electrode is maintained at a furnace temperature ranging from 600 to 850 DEG C; (8) the Ag inner multilayer ceramic capacitor is obtained after the terminal electrode is baked and cooled down. The method for preparing Ag inner electrode multilayer ceramic capacitors is characterized by simple preparation process, small dielectric loss and good stability, the prepared multilayer ceramic capacitor has high withstand voltage strength, high dielectric constant, capacitor temperature change rate in conformity with the NPO feature standards.

Description

The method for preparing Ag inner electrode multilayer ceramic capacitors
Technical field
The present invention relates to technical field of ceramic material, particularly prepare the method for Ag inner electrode multilayer ceramic capacitors.
Background technology
Multilayer ceramic capacitor (Multilayer Ceramic Capacitors) is called for short MLCC, and it is electrode material and ceramic body to be replaced, joins with multilayer fold and burn till an integral body.Microminiaturization, chip type along with ceramic electron element, the number of plies of circuit, interior electrode rapidly increases in the space of the same volume of chip component, be in the chip component in the shared proportion of the cost of electrode increasing, this objectively just require the inner electrode of lamination sheet type element must be gradually by the very high platinum of cost, platinum silver electrode then change by lower-cost fine silver electrode and replace.But electrode has brought other problem in the fine silver, and the fusing point of fine silver electrode is 960 ℃, and promptly the ceramic powder that burns altogether with the fine silver electrode must sinter porcelain under less than 960 ℃ cryogenic conditions.At present, has the ceramic material of the NPO characteristic (the NPO characteristic promptly is meant-55～125 ℃ | TCC|＜=30ppm/ ℃) of the international EIA of Electronic Industries Association regulation, basically by BaO-Ln 2O 3-TiO 2Series ceramic material and Bi 2O 3-ZnO/CaO-Nb 2O 5Series ceramic material constitutes, and the former application is relatively more extensive.The densification firing temperature of BaLnTi series ceramic material itself is generally more than 1250 ℃, can realize in the prior art that low sintering this type of porcelain all is to help at the low temperature that the BaLnTi based material has mixed vast scale to burn glass or other compounds basically, burns the dielectric constant that auxiliary material adds the very big reduction porcelain of affiliation and help in a large number.BaO-Ln at 850～1000 ℃ of temperature range sintering 2O 3-TiO 2The dielectric constant of ternary system porcelain all is to be in 20～70 scope basically; And the doping of the frit of its big content also influences the temperature stability and the withstand voltage properties of porcelain.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the purpose of this invention is to provide a kind of method for preparing Ag inner electrode multilayer ceramic capacitors.It has, and preparation technology is simple, dielectric loss is little, the characteristics of good stability, the multilayer ceramic capacitor compressive resistance height, the dielectric constant height that make, and temperature coefficient of capacitance satisfies the NPO characteristic standard.
In order to reach the foregoing invention purpose, technical scheme of the present invention realizes as follows:
Prepare the method for Ag inner electrode multilayer ceramic capacitors, the steps include:
1. batch mixing: with major ingredient aBaO-bLn 2O 3-cBi 2O 3-dTiO 2(be abbreviated as BLT, wherein Ln is a lanthanide series rare-earth elements) and auxiliary material eBi 2O 3-fB 2O 3-gZnO-hSiO 2(being abbreviated as BBZS) glass one and jBaO-kLi 2O-lCaO-mSrO-nSiO 2(being abbreviated as BLCS) glass two is mixed into compound, and adds deionization aqueous solvent ball milling 2～48 hours;
2. oven dry: the compound behind the oven dry ball milling;
3. curtain coating: the compound after will drying mixes with organic solvent and ball milling 2～48 hours, become dielectric layer according to the organic ink curtain coating of casting technique after with ball milling, type metal Ag inner electrode on dielectric layer makes dielectric layer and Ag inner electrode mutual superposition form the green compact of multilayer ceramic capacitor simultaneously;
4. binder removal: green compact are incubated 2～20 hours in air under 300 ℃ temperature;
5. sintering: green compact are sintering in air, and sintering temperature is at 850～950 ℃;
6. cooling: the green compact behind the sintering naturally cool to room temperature in air;
7. termination electrode: Ag inner electrode is incubated 1～2 hour as the green compact of termination electrode in 600～850 ℃ of furnace temperature;
8. moulding: termination electrode obtains Ag inner electrode multilayer ceramic capacitors after baking cooling.
In said method, described major ingredient aBaO-bLn 2O 3-cBi 2O 3-dTiO 2In each molar ratio coefficient a, b, c and d satisfy following condition: a+b+c+d=1,0.13≤a≤0.17; 0.12≤b≤0.22; 0.01≤c≤0.1; 0.4≤d≤0.74.
In said method, eBi in the described auxiliary material 2O 3-fB 2O 3-gZnO-hSiO 2Glass one each percentage by weight e, f, g and h satisfy following condition: e+f+g+h=100,50≤e≤90; 5≤f≤30; 4≤g≤30; 1≤h≤20.JBaO-kLi in the auxiliary material 2O-lCaO-mSrO-nSiO 2Glass two each percentage by weight j, k, l, m and n satisfy following condition: j+k+l+m+n=100,20≤j≤25,5≤k≤10,5≤l≤10,0≤m≤10,50≤n≤70.
In said method, described major ingredient aBaO-bLn 2O 3-cBi 2O 3-dTiO 2Weight percentage in compound is 90～99wt%.The weight percentage of auxiliary material in compound is 1～10wt%, wherein glass one eBi 2O 3-fB 2O 3-gZnO-hSiO 2Weight percentage in auxiliary material is 70～90wt%, glass two jBaO-kLi 2O-lCaO-mSrO-nSiO 2Weight percentage in auxiliary material is 10～30wt%.
The present invention has been owing to adopted said method, the green compact of multilayer ceramic capacitor with silver metal as the internal electrode material, can be at the sintering temperature that is lower than silver point and densification.As the dielectric material of capacitor main body in densification process and Ag inner electrode can be good common burning and do not produce significant silver electrode process of osmosis.The present invention has that preparation technology is simple, dielectric loss is little, the characteristics of good stability.The multilayer ceramic capacitor that makes has not only had splendid NPO characteristic, simultaneously can also keep very high dielectric constant under low sintering condition, and poisonous elements such as not leaded in the material, cadmium and arsenic.
The present invention will be further described below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the stereoscan photograph of the embodiment of the invention 1 sample surfaces pattern;
Fig. 2 is the stereoscan photograph of the embodiment of the invention 2 sample surfaces patterns;
Fig. 3 is the stereoscan photograph of the embodiment of the invention 3 sample surfaces patterns.
Embodiment
Used major ingredient was by aBaO-bLn when the present invention prepared 2O 3-cBi 2O 3-dTiO 2The composition of expression, wherein a, b, c and d independently represent molar ratio respectively, satisfy: a+b+c+d=1,0.13≤a≤0.17; 0.12≤b≤0.22; 0.01≤c≤0.1; 0.4≤d≤0.74.The initiation material that is used to make the ceramic powder major ingredient is not limited to the oxide of each element, can use the carbonate that respectively constitutes element, nitrate, replacements such as organic metal salt.Preferably the purity of each initiation material is not still done special restriction all greater than more than 99% yet.The initiation material of major ingredient can adopt BaCO 3, Nd 2O 3, Bi 2O 3And TiO 2Powder.According to the prescription each raw material of molal quantity proportioning weighing, with water as each initiation material of solvent.With compound ball milling 2～48 hours, make slurry before the pre-burning.With after the slurry oven dry, in 1100 ℃ alumina crucible, calcined base-material powder behind the synthesis pre-burning 1～10 hour then.The base-material powder is crushed to average grain diameter＜1 μ m with barreling or other ball-milling technology with it again, has just made the BLT material of the key component in the required ceramic material.
EBi in the auxiliary material glass compound of using among the present invention 2O 3-fB 2O 3-gZnO-hSiO 2Each percentage by weight e, f, g and the h of glass one satisfy following condition: e+f+g+h=100,50≤e≤90; 5≤f≤30; 4≤g≤30; 1≤h≤20.At first choose the oxide material of respective element according to the percentage by weight of prescription decision, each initiation material of weighing is a solvent with ethanol then, adopts ball-milling technology that each raw material is mixed 2～48 hours preparation slurries.Then with slurry oven dry, at 900～1100 ℃ temperature lower calcination, treat its fusion after, the glass compound of molten condition is obtained glass blocks through water-cooled.By ball-milling technology the glass blocks that obtains is crushed to the granularity of regulation at last, promptly obtains glass one powder in the auxiliary material.JBaO-kLi 2O-lCaO-mSrO-nSiO 2Each percentage by weight j, k, l, m and the n of glass two satisfy following condition: j+k+l+m+n=100,20≤j≤25,5≤k≤10,5≤l≤10,0≤m≤10,50≤n≤70.At first choose the oxide material of respective element according to the percentage by weight of prescription decision, each initiation material of weighing, be each initiation material of solvent and ball milling 2～48 hours then with ethanol, make slurry, slurry oven dry back is become the glass compound of molten condition at 1400～1450 ℃ temperature lower calcination, the glass compound of molten condition is obtained glass blocks through water-cooled, glass blocks is pulverized obtained glass two powders in the auxiliary material.Weighing glass one powder and glass two powders are that solvent glass one powder and glass two powders and ball milling closed 2～48 hours with ethanol by weight ratio, make slurry, and the slurry oven dry is made the auxiliary material powder;
The method for preparing Ag inner electrode multilayer ceramic capacitors with above-mentioned ceramic powder is as follows:
1. batch mixing: with major ingredient aBaO-bLn 2O 3-cBi 2O 3-dTiO 2With auxiliary material eBi 2O 3-fB 2O 3-gZnO-hSiO 2Glass one and jBaO-kLi 2O-lCaO-mSrO-nSiO 2Glass two is mixed into compound, and adds the solvent deionized water ball milling 2～48 hours;
2. oven dry: the compound behind the oven dry ball milling;
3. curtain coating: the compound after will drying mixes with organic solvent and ball milling 2～48 hours, become dielectric layer according to the organic ink curtain coating of casting technique after with ball milling, type metal Ag inner electrode on dielectric layer makes dielectric layer and Ag inner electrode mutual superposition form the multilayer ceramic capacitor green compact simultaneously;
4. binder removal: the multilayer ceramic capacitor green compact are incubated 2～20 hours in air under 300 ℃ temperature;
5. sintering: green compact are sintering in air, and sintering temperature is at 850～950 ℃;
6. cooling: the green compact behind the sintering naturally cool to room temperature in air;
7. termination electrode: Ag inner electrode is incubated 1～2 hour as the green compact of termination electrode in 600～850 ℃ of furnace temperature;
8. termination electrode obtains Ag inner electrode multilayer ceramic capacitors after baking cooling.
Embodiment 1
Raw material in the major ingredient BLT ceramic material adopts BaCO 3, Nd 2O 3, Bi 2O 3And TiO 2, wherein each material composition is according to BaCO 3: 15.0ml%; Nd 2O 3: 14.54ml%; Bi 2O 3: 3.19ml%; TiO 2: the weighing of 67.22ml% proportioning.Make the major ingredient powder through behind ball milling, oven dry and the calcine technology.Auxiliary material B BZS glass one and BLCS glass two mixture powders, its raw material adopts Bi respectively 2O 3, B 2O 3, ZnO and SiO 2And BaO, Li 2O, CaO, SrO and SiO 2Wherein BBZS glass one each material composition is according to Bi 2O 3: 83.17wt%; B 2O 3: 6.55wt%; ZnO:9.05wt%; SiO 2: the weighing of 1.23wt% proportioning, BLCS glass two each material compositions are according to BaO:24.26wt%; Li 2O:8.8wt%; CaO:12.14wt%; SrO:0.0wt%; SiO 2: the weighing of 54.8wt% proportioning.After glass one powder and glass two powders process ball milling, oven dry and glassification process, carry out the mixing of two kinds of frits once more, mixed weight percentage is BBZS:90wt%; BLCS:10wt% makes the auxiliary material powder.Then with above-mentioned major ingredient powder and auxiliary material powder according to mass ratio (BBZS+BLCS): the proportioning of BLT=60% is mixed, ball milling, the dry porcelain that obtains.The casting film-forming sheet superposes alternately with Ag inner electrode then, makes the MLCC green compact, behind the binder removal, 940 ℃ of sintered heat insulatings 3 hours, bakes the Ag termination electrode then and makes multilayer ceramic capacitor MLCC sample, as shown in Figure 1.This multilayer ceramic capacitor MLCC sample is carried out the test of dielectric property, and dielectric property are referring to table 1.
Sample Sintering condition Dielectric constant (25 ℃) ??TCC??ppm/℃ ??tgδ??x10 -4 ??ρ(25℃)??Ω.cm ??E br(25℃)??KV/mm
??1 ??920℃/3h ??89 ??-3.1 ??5 ??4.4x10 13 ??15.2
Table 1
Embodiment 2
Raw material in the major ingredient BLT ceramic material adopts BaCO 3, Nd 2O 3, Bi 2O 3And TiO 2, wherein each material composition is according to BaCO 3: 15.05ml%; Nd 2O 3: 14.54ml%; Bi 2O 3: 3.19ml%; TiO 2: the weighing of 67.22ml% proportioning.Make the major ingredient powder through behind ball milling, oven dry and the calcine technology.Auxiliary material B BZS glass one and BLCS glass two mixture powders, its raw material adopts Bi respectively 2O 3, B 2O 3, ZnO and SiO 2And BaO, Li 2O, CaO, SrO and SiO 2Wherein BBZS glass one each material composition is according to Bi 2O 3: 76.72wt%; B 2O 3: 9.05wt%; ZnO:12.52wt%; SiO 2: the weighing of 1.71wt% proportioning, BLCS glass two each material compositions are according to BaO:24.26wt%; Li 2O:8.8wt%; CaO:12.14wt%; SrO:0.0wt%; SiO 2: the weighing of 54.8wt% proportioning.After glass one powder and glass two powders process ball milling, oven dry and glassification process, carry out the mixing of two kinds of frits once more, mixed weight percentage is BBZS:75wt%; BLCS:25wt% makes the auxiliary material powder.Then with above-mentioned major ingredient powder and auxiliary material powder according to mass ratio (BBZS+BLCS): the proportioning of BLT=60% is mixed, ball milling, the dry porcelain that obtains.The casting film-forming sheet superposes alternately with Ag inner electrode then, makes the MLCC green compact, behind the binder removal, 940 ℃ of sintered heat insulatings 3 hours, bakes the Ag termination electrode then and makes multilayer ceramic capacitor MLCC sample, as shown in Figure 2.This multilayer ceramic capacitor MLCC sample is carried out the test of dielectric property, and dielectric property are referring to table 2.
Sample Sintering condition Dielectric constant (25 ℃) ??TCC??ppm/℃ ??tgδ??x10 -4 ??ρ(25℃)??Ω.cm ??E br(25℃)??KV/mm
??2 ??940℃/3h ??88 ??-7.0 ??5 ??3.2x10 13 ??15.1
Table 2
Embodiment 3
Raw material in the major ingredient BLT ceramic material adopts BaCO 3, Nd 2O 3, Bi 2O 3And TiO 2, wherein each material composition is according to BaCO 3: 15.16ml%; Nd 2O 3: 14.65ml%; Bi 2O 3: 3.22ml%; TiO 2: the weighing of 66.97ml% proportioning.Through making the powder body material of key component behind ball milling, oven dry and the calcine technology.Auxiliary material B BZS glass one and BLCS glass two mixture powders, its raw material adopts Bi respectively 2O 3, B 2O 3, ZnO and SiO 2And BaO, Li 2O, CaO, SrO and SiO 2Wherein BBZS glass one each material composition is according to Bi 2O 3: 70.66wt%; B 2O 3: 12.84wt%; ZnO:14.08wt%; SiO 2: the weighing of 2.42wt% proportioning, BLCS glass two each material compositions are according to BaO:23.13wt%; Li 2O:8.8wt%; CaO:9.39wt%; SrO:3.48wt%; SiO 2: the weighing of 55.2wt% proportioning.After glass one powder and glass two powders process ball milling, oven dry and glassification process, carry out the mixing of two kinds of frits once more, mixed weight percentage is BBZS:75wt%; BLCS:25wt% makes the auxiliary material powder.Then with above-mentioned major ingredient powder and auxiliary material powder according to mass ratio (BBZS+BLCS): the proportioning of BLT=80% is mixed, ball milling, the dry porcelain that obtains.The casting film-forming sheet superposes alternately with Ag inner electrode then, makes the MLCC green compact, behind the binder removal, 940 ℃ of sintered heat insulatings 3 hours, bakes the Ag termination electrode then and makes multilayer ceramic capacitor MLCC sample, as shown in Figure 3.This multilayer ceramic capacitor MLCC sample is carried out the test of dielectric property, and dielectric property are referring to table 3.
Sample Sintering condition Dielectric constant (25 ℃) ??TCC??ppm/℃ ??tgδ??x10 -4 ??ρ(25℃)??Ω.cm ??E br(25℃)??Kv/mm
??3 ??900℃/3h ??89 ??-15.2 ??5 ??1.8x10 13 ??15.5
Table 3
The foregoing description has prepared the ceramic material of the high-k Ag inner electrode MLCC of satisfied temperature offset-type NPO type standard performance index in 850～1000 ℃ temperature range, the room temperature dielectric constant of MLCC is controlled between 80～90, and dielectric loss is less than 10 -3, compressive resistance is greater than 15Kv/mm.Use sintering method of the present invention, but can obtain high-k, high compressive resistance low-temperature sintering, be the dielectric ceramic material of the temperature compensating type NPO characteristic MLCC of interior electrode with silver.

Claims (4)

1. prepare the method for Ag inner electrode multilayer ceramic capacitors, the steps include:
1. batch mixing: with major ingredient aBaO-bLn 2O 3-cBi 2O 3-dTiO 2With auxiliary material eBi 2O 3-fB 2O 3-gZnO-hSiO 2Glass one and jBaO-kLi 2O-lCaO-mSrO-nSiO 2Glass two is mixed into compound, and adds the deionized water solvent ball milling 2～48 hours;
2. oven dry: the compound behind the oven dry ball milling;
3. curtain coating: the compound after will drying mixes with organic solvent and ball milling 2～48 hours, become dielectric layer according to the organic ink curtain coating of casting technique after with ball milling, type metal Ag inner electrode on dielectric layer makes dielectric layer and Ag inner electrode mutual superposition form the green compact of multilayer ceramic capacitor simultaneously;
4. binder removal: green compact are incubated 2～20 hours in air under 300 ℃ temperature;
5. sintering: green compact are sintering in air, and sintering temperature is at 850～950 ℃;
6. cooling: the green compact behind the sintering naturally cool to room temperature in air;
7. termination electrode: Ag inner electrode is incubated 1～2 hour as the green compact of termination electrode in 600～850 ℃ of furnace temperature;
8. moulding: termination electrode obtains Ag inner electrode multilayer ceramic capacitors after baking cooling.
2. the method for preparing Ag inner electrode multilayer ceramic capacitors according to claim 1 is characterized in that, described major ingredient aBaO-bLn 2O 3-cBi 2O 3-dTiO 2In each molar ratio coefficient a, b, c and d satisfy following condition: a+b+c+d=1,0.13≤a≤0.17; 0.12≤b≤0.22; 0.01≤c≤0.1; 0.4≤d≤0.74.
3. the method for preparing Ag inner electrode multilayer ceramic capacitors according to claim 1 is characterized in that, eBi in the described auxiliary material 2O 3-fB 2O 3-gZnO-hSiO 2Glass one each percentage by weight e, f, g and h satisfy following condition: e+f+g+h=100,50≤e≤90; 5≤f≤30; 4≤g≤30; 1≤h≤20; JBaO-kLi in the auxiliary material 2O-lCaO-mSrO-nSiO 2Glass two each percentage by weight j, k, l, m and n satisfy following condition: j+k+l+m+n=100,20≤j≤25,5≤k≤10,5≤l≤10,0≤m≤10,50≤n≤70.
4. according to claim 1, the 2 or 3 described methods that prepare Ag inner electrode multilayer ceramic capacitors, it is characterized in that described major ingredient aBaO-bLn 2O 3-cBi 2O 3-dTiO 2Weight percentage in compound is 90～99wt%; The weight percentage of auxiliary material in compound is 1～10wt%, wherein glass one eBi 2O 3-fB 2O 3-gZnO-hSiO 2Weight percentage in auxiliary material is 70～90wt%, glass two jBaO-kLi 2O-lCaO-mSrO-nSiO 2Weight percentage in auxiliary material is 10～30wt%.
CN200810239688A 2008-12-15 2008-12-15 Method for preparing Ag inner electrode multilayer ceramic capacitors Pending CN101752082A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104193349A (en) * 2014-08-26 2014-12-10 东莞市戍普电子科技有限公司 Glass powder applicable to NPO ceramic body as well as preparation method and application of glass powder

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104193349A (en) * 2014-08-26 2014-12-10 东莞市戍普电子科技有限公司 Glass powder applicable to NPO ceramic body as well as preparation method and application of glass powder

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