CN1420105A - Dielectric ceramic material, preparation method thereof and method for producing ceramic capacitor - Google Patents
Dielectric ceramic material, preparation method thereof and method for producing ceramic capacitor Download PDFInfo
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- CN1420105A CN1420105A CN 02151904 CN02151904A CN1420105A CN 1420105 A CN1420105 A CN 1420105A CN 02151904 CN02151904 CN 02151904 CN 02151904 A CN02151904 A CN 02151904A CN 1420105 A CN1420105 A CN 1420105A
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Abstract
A ceramic medium is prepared from the composite, oxide, MgaCab SrcBa1-a-b-cZrdO1+2d, where a=0-1, b=0-1, c=0-1 and d=0.8-1.2, through ball grinding, drying, pulverizing, calcining at 1200-1300 deg.C for 2-3 hr, adding sintering aid, pulverizing, and sintering. It can be used to prepare multi-layer capacitor using Ni or Ni-alloy as internal electrodes.
Description
Technical field
The present invention relates to a kind of anti-reduction heat and stablize ceramic medium material.
The invention still further relates to above-mentioned anti-reduction heat and stablize the preparation method of ceramic medium material.
The invention still further relates to method with above-mentioned material produce multiple-layer sheet ceramic capacitor.
Background technology
Multiple-layer sheet ceramic capacitor is with its small volume, high reliability and mount characteristics such as convenient and be used widely in the manufacturing processed of electronics.Along with the development and the arrival in mobile communication epoch of digitizing technique, various electron devices and equipment require surface-pasted multiple-layer sheet ceramic capacitor to realize small size, large vol and high reliability to miniaturization, the development of high-density integrated direction.
Multiple-layer sheet ceramic capacitor is to pass through screen printing technique, the pulp layer of electrode in forming is printed on the medium layer, alternative stacked, and through compacting, cutting back formation green compact, again base substrate and interior electrode are at high temperature burnt altogether, end-blocking electrode slurry, the element of making through Overheating Treatment more subsequently with internal and external electrode.
Traditional multiple-layer sheet ceramic capacitor is an agglomerating in air atmosphere.Not oxidized in the process of high temperature co-firing for electrode in making, the slurry of interior electrode adopts the precious metal palladium silver alloys traditionally.Because it is high that the market value of precious metal palladium continues, the manufacturing cost of traditional multiple-layer sheet ceramic capacitor is also high.
If with base metal nickel or nickelalloy interior electrode as multiple-layer sheet ceramic capacitor, oxidized for electrode in preventing, must in reducing atmosphere, carry out sintering processes.But traditional multiple-layer sheet ceramic capacitor has with dielectric material that sintering is reduced into semi-conductive characteristic under reducing atmosphere, can not satisfy with base metal nickel or nickelalloy and make requirement as the multiple-layer sheet ceramic capacitor of interior electrode.
Summary of the invention
The objective of the invention is provides a kind of anti-reduction heat to stablize ceramic medium material at above deficiency.
The invention still further relates to above-mentioned anti-reduction heat and stablize the preparation method of ceramic medium material, can have the high frequency heat stable ceramic medium material of anti-reduction characteristic at agglomerating under the reducing atmosphere.
The invention still further relates to method with above-mentioned material produce multiple-layer sheet ceramic capacitor.
The principal constituent that a kind of anti-reduction heat provided by the invention is stablized preparation method's employing of ceramic medium material is the composite oxides that comprise Mg, Ca, Sr, Ba metallic element and Zr and O element, with formula Mg
aCa
bSr
cBa
1-a-b-cZr
dO
1+2dExpression, 0≤a in the formula≤1,0≤b≤1,0≤c≤1,0.8≤d≤1.2; Based on this principal constituent, this ceramic medium material can also comprise ZnO, the SiO of 0.1～5%mol
2, MnO
2, K
2O wherein one or more, as sintering aid; Calcined 2-3 hour at 1200 ℃ to 1300 ℃ after the refinement of principal constituent process wet ball grinding, drying, the pulverizing, add sintering aid, be crushed to the powder average particulate diameter less than 1 μ m, 1250～1350 ℃ sinter to material dielectric constant between 20 to 40 in the nitrogen and hydrogen mixture atmosphere, temperature factor is 0 ± 30PPM/ ℃, meets EIA standard C OG temperature profile.
Using the method for giving an account of material production multiple-layer sheet ceramic capacitor comprises:
(1) after the traditional casting technique of employing is produced the diaphragm of 5～100 μ m, adopt electrode in the screen printing technique double exposure, repressed again, cutting forms green compact;
(2) with green compact 1250～1350 ℃ of sintering in the nitrogen and hydrogen mixture atmosphere, after handling through surface finish again, envelope copper alloy or nickelalloy terminal electrode paste;
(3) after 800～900 ℃ of thermal treatments of nitrogen atmosphere, handle through three layers of electroplating technology, form the end electrode of copper-nickel-Xi or nickel-nickel-Xi structure.
In (1) step, electrode size can use the nickelalloy slurry that contains 0.1～10% inorganic additive.
In (3) step, terminal electrode paste can use copper alloy or the nickelalloy slurry that contains 1～20% inorganic additive.
The specific inductivity of this multiple-layer sheet ceramic capacitor is between 20 to 40, and temperature factor is 0 ± 30PPM/ ℃ and meets EIA standard C OG temperature profile.
The present invention compared with prior art has following advantage:
1, this stupalith can be made the medium layer that thickness is 5-10 μ m;
2, this stupalith alkalescence is low, and therefore wideer technology tolerance is arranged;
3, this stupalith has little loss tangent and good electric durability energy;
4, this stupalith has high insulation resistance.
Embodiment
Introduce specific embodiments of the present invention below in conjunction with embodiment.
Embodiment 1
The present embodiment is mainly introduced the preparation process that anti-reduction heat is stablized ceramic medium material, forms and characteristic.
Preparation process comprises the preparation of principal constituent and the preparation of ceramic dielectic powder.
The preparation process of principal constituent comprises: with initial starting material such as MgCO
3, CaCO
3, SrCO
3, BaCO
3And ZrO
2By formula Mg
aCa
bSr
cBa
1-a-b-cZr
dO
1+2dThe ratio weighing join part, a, b, c and d list in table 1 in the formula.Through calcining 2 to 3 hours at 1200 ℃ to 1300 ℃ after wet ball grinding refinement, drying, the pulverizing, obtain required principal constituent again.
The preparation process of ceramic dielectic powder is: add auxiliary component as sintering aid in principal constituent, the quality percentage composition of each auxiliary component is listed in table 1.After mixing through ball milling, again by the processing of technology such as superfine grinding and classification, get final product average particulate diameter less than the ceramic powder of 1 μ m.
Granulation behind the adding PVA tamanori in this ceramic dielectic powder, and be pressed into diameter 15mm, the disk sample green compact of the about 1mm of thickness.With sample green compact 1250～1350 ℃ of sintering in the nitrogen and hydrogen mixture atmosphere, be coated with the copper alloy terminal electrode paste on two surfaces up and down again, and after 800～900 ℃ of thermal treatments of nitrogen atmosphere, with alcohol wash, dry.Use its performance of correlate meter testing of equipment then, each sample performance is listed in table 2.
Table 1
| Sample | Principal constituent (Mg aCa bSr cBa 1-a-b-cZr dO 1+2d) form | The quality percentage composition (wt%) of each auxiliary component | ||||||
| ??a | ??b | ??c | ??d | ??ZnO | ??SiO 2 | ??MnO 2 | ??K 2O | |
| ??1 | ??0.10 | ??0.30 | ??0.50 | ??1.00 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??2 | ??0.10 | ??0.30 | ??O.50 | ??0.90 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??3 | ??0.10 | ??0.30 | ??0.50 | ??1.10 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??4 | ??0.10 | ??0.30 | ??0.50 | ??1.00 | ??0.15 | ??0.65 | ??0.10 | ??0.05 |
| ??5 | ??0.10 | ??0.30 | ??0.50 | ??1.00 | ??0.30 | ??0.30 | ??0.10 | ??0.05 |
| ??6 | ??0.10 | ??0.30 | ??0.50 | ??1.00 | ??0.20 | ??0.40 | ??0.10 | ??0.00 |
| ??7 | ??0.05 | ??0.80 | ??0.10 | ??1.00 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??8 | ??0.05 | ??0.80 | ??0.10 | ??0.90 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??9 | ??0.05 | ??0.80 | ??0.10 | ??1.10 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??10 | ??0.20 | ??0.70 | ??0.05 | ??1.00 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??11 | ??0.20 | ??0.70 | ??0.05 | ??0.90 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??12 | ??0.20 | ??0.70 | ??0.05 | ??1.10 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??13 | ??0.05 | ??0.30 | ??0.20 | ??1.00 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??14 | ??0.05 | ??0.30 | ??0.20 | ??0.90 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
| ??15 | ??0.05 | ??0.30 | ??0.20 | ??1.10 | ??0.20 | ??0.40 | ??0.10 | ??0.05 |
Table 2
| Sample | Sintering temperature (℃) | Specific inductivity | Loss tangent | Temperature factor (PPM/ ℃) | Resistivity (Ω .cm) |
| ????1 | ????1300 | ????30 | ??3×10 -4 | ????10 | ????＞10 13 |
| ????2 | ????1300 | ????30 | ??5×10 -4 | ????10 | ????＞10 13 |
| ????3 | ????1300 | ????30 | ??2×10 -4 | ????10 | ????＞10 13 |
| ????4 | ????1260 | ????30 | ??4×10 -4 | ????10 | ????＞10 13 |
| ????5 | ????1330 | ????30 | ??5×10 -4 | ????10 | ????＞10 13 |
| ????6 | ????1340 | ????30 | ??5×10 -4 | ????10 | ????＞10 13 |
| ????7 | ????1300 | ????28 | ??3×10 -4 | ????-20 | ????＞10 13 |
| ????8 | ????1300 | ????28 | ??4×10 -4 | ????-20 | ????＞10 13 |
| ????9 | ????1300 | ????28 | ??4×10 -4 | ????-20 | ????＞10 13 |
| ????10 | ????1300 | ????22 | ??3×10 -4 | ????0 | ????＞10 13 |
| ????11 | ????1300 | ????22 | ??4×10 -4 | ????0 | ????＞10 13 |
| ????12 | ????1300 | ????22 | ??2×10 -4 | ????0 | ????＞10 13 |
| ????13 | ????1300 | ????38 | ??5×10 -4 | ????20 | ????＞10 13 |
| ????14 | ????1300 | ????38 | ??4×10 -4 | ????20 | ????＞10 13 |
| ????15 | ????1300 | ????38 | ??3×10 -4 | ????20 | ????＞10 13 |
By table 2 as seen, anti-reduction ceramic medium material of the present invention is suitable for sintering in the nitrogen and hydrogen mixture atmosphere, and sintering temperature is between 1250 ℃ to 1350 ℃, and specific inductivity is between 20 to 40, and loss tangent is less than 5 * 10
-4, resistivity is greater than＞10
13Ω .cm, temperature factor meets EIA standard C OG temperature profile between-30PPM/ ℃ to+30PPM/ ℃.
Embodiment 2
The present embodiment is mainly introduced the thermally-stabilised multiple-layer sheet ceramic capacitor of nickel inner electrode copper termination (MLCC) preparation process and characteristic thereof.
Its characteristics be it with embodiment 1 described anti-reduction ceramic medium material as dielectric material, electrode size uses the nickelalloy slurry contain 0.1～10% inorganic additive, and terminal electrode paste uses the copper alloy slurry that contains 1～20% inorganic additive.
The thermally-stabilised multiple-layer sheet ceramic capacitor of nickel inner electrode (MLCC) preparation process that the present embodiment is introduced comprises:
After adopting traditional casting technique to produce the diaphragm of 5～100 μ m, adopt screen printing technique, the above-mentioned nickelalloy electrode size that contains 0.1～10% inorganic additive is printed on the diaphragm, and alternative stacked, to form electrode in the multilayer.Repressed again, cutting forms green compact.The used tamanori of curtain coating slurrying is not a key of the present invention, can select from tamanori commonly used, can use novel water-based adhesive yet.
Green compact are carried out binder removal again and handle in nitrogen, preferred processing condition is: be warming up to 300～450 ℃ with 60～100 ℃ speed per hour, be incubated 10-40 hour again.
(oxygen partial pressure is less than 10 in the nitrogen and hydrogen mixture atmosphere with the green compact after the binder removal processing
-6Atm) 1250～1350 ℃ sintering 2-3 hour, after handling through surface finish, again with the above-mentioned copper alloy terminal electrode paste end-blocking that contains 1～20% inorganic additive.And under nitrogen atmosphere, after 800～900 ℃ of thermal treatment, handle through three layers of electroplating technology, form the end electrode of copper-nickel-Xi structure.
Multiple-layer sheet ceramic capacitor (MLCC) by above-mentioned technology is made can be 0201,0603,0805,1206,1812 equidimension specifications, and nominal capacity is at 0.1PF to 10, between the 000PF.Loss tangent is less than 5 * 10
-4, insulation resistance is greater than 10
11Ω, proof voltage is greater than 1000V
DC, temperature factor-30PPM/ ℃ to+30PPM/ ℃, meet EIA standard C OG temperature profile.
Embodiment 3
The present embodiment is mainly introduced nickel inner electrode nickel nickel end electrode thermally-stabilised multiple-layer sheet ceramic capacitor (MLCC) preparation process and characteristic thereof.
Its characteristics be it with embodiment 1 described anti-reduction ceramic medium material as dielectric material, electrode size uses the nickelalloy slurry contain 0.1～10% inorganic additive, and terminal electrode paste uses the nickelalloy slurry that contains 1～20% inorganic additive.
The thermally-stabilised multiple-layer sheet ceramic capacitor of nickel inner electrode (MLCC) preparation process that the present embodiment is introduced comprises:
After adopting traditional casting technique to produce the diaphragm of 5～100 μ m, adopt screen printing technique, the above-mentioned nickelalloy electrode size that contains 0.1～10% inorganic additive is printed on the diaphragm, and alternative stacked, to form electrode in the multilayer.Repressed again, cutting forms green compact.The used tamanori of curtain coating slurrying is not a key of the present invention, can select from tamanori commonly used, can use novel water-based adhesive yet.
Green compact are carried out binder removal again and handle in nitrogen, preferred processing condition is: be warming up to 300～450 ℃ with 60～100 ℃ speed per hour, be incubated 10-40 hour again.
(oxygen partial pressure is less than 10 in the nitrogen and hydrogen mixture atmosphere with the green compact after the binder removal processing
-6Atm) 1250～1350 ℃ sintering 2-3 hour, after handling through surface finish, again with the above-mentioned nickelalloy terminal electrode paste end-blocking that contains 1～20% inorganic additive.And under nitrogen atmosphere, after 800～900 ℃ of thermal treatment, handle through three layers of electroplating technology, form the end electrode of nickel-nickel-Xi structure.
Multiple-layer sheet ceramic capacitor (MLCC) by above-mentioned technology is made can be 0201,0603,0805,1206,1812 equidimension specifications, and nominal capacity is at 0.1PF to 10, between the 000PF.Loss tangent is less than 5 * 10
-4, insulation resistance is greater than 10
11Ω, proof voltage is greater than 1000V
DC, temperature factor-30PPM/ ℃ to+30PPM/ ℃, meet EIA standard C OG temperature profile.
Claims (6)
1, a kind of anti-reduction heat is stablized the preparation method of ceramic medium material, it is characterized in that the principal constituent that adopts is the composite oxides that comprise Mg, Ca, Sr, Ba metallic element and Zr and O element, with formula Mg
aCa
bSr
cBa
1-a-b-cZr
dO
1+2dExpression, 0≤a in the formula≤1,0≤b≤1,0≤c≤1,0.8≤d≤1.2; Based on this principal constituent, this ceramic medium material can also comprise ZnO, the SiO of 0.1～5%mol
2, MnO
2, K
2O wherein one or more, as sintering aid; Calcined 2-3 hour at 1200 ℃ to 1300 ℃ after the refinement of principal constituent process wet ball grinding, drying, the pulverizing, add sintering aid, be crushed to the powder average particulate diameter less than 1 μ m, 1250～1350 ℃ sinter to material dielectric constant between 20 to 40 in the nitrogen and hydrogen mixture atmosphere, temperature factor is 0 ± 30PPM/ ℃, meets EIA standard C OG temperature profile.
2, the anti-reduction heat of the described method preparation of claim 1 is stablized ceramic medium material.
3, stablize the method that ceramic medium material is produced multiple-layer sheet ceramic capacitor with the described anti-reduction heat of claim 2, it is characterized in that comprising:
(1) after the traditional casting technique of employing is produced the diaphragm of 5～100 μ m, adopt electrode in the screen printing technique double exposure, repressed again, cutting forms green compact;
(2) with green compact 1250～1350 ℃ of sintering in the nitrogen and hydrogen mixture atmosphere, after handling through surface finish again, envelope copper alloy or nickelalloy terminal electrode paste;
(3) after 800～900 ℃ of thermal treatments of nitrogen atmosphere, handle through three layers of electroplating technology, form the end electrode of copper-nickel-Xi or nickel-nickel-Xi structure.
4, production method according to claim 3 is characterized in that electrode size can use the nickelalloy slurry that contains 0.1～10% inorganic additive in (1) step.
5,, it is characterized in that terminal electrode paste can use copper alloy or the nickelalloy slurry that contains 1～20% inorganic additive in (3) step according to claim 3 or 4 described production methods.
6, the multiple-layer sheet ceramic capacitor of the described method production of claim 3 is characterized in that its specific inductivity between 20 to 40, and temperature factor is 0 ± 30PPM/ ℃ and meets EIA standard C OG temperature profile.
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|---|---|---|---|
| CN 02151904 CN1211316C (en) | 2002-11-08 | 2002-11-08 | Dielectric ceramic material, preparation method thereof and method for producing ceramic capacitor |
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|---|---|---|---|
| CN 02151904 CN1211316C (en) | 2002-11-08 | 2002-11-08 | Dielectric ceramic material, preparation method thereof and method for producing ceramic capacitor |
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| Publication Number | Publication Date |
|---|---|
| CN1420105A true CN1420105A (en) | 2003-05-28 |
| CN1211316C CN1211316C (en) | 2005-07-20 |
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863221A (en) * | 2012-09-20 | 2013-01-09 | 广东风华高新科技股份有限公司 | Method, sintering aid and materials for preparation of low-temperature cofired medium ceramic and application |
| CN103295780A (en) * | 2013-06-20 | 2013-09-11 | 广东风华高新科技股份有限公司 | Manufacturing method for multi-layer ceramic capacitor |
| CN103922714A (en) * | 2014-03-18 | 2014-07-16 | 福建火炬电子科技股份有限公司 | Low dielectric constant multi-layer capacitor ceramic material and preparation method thereof |
| CN104761257A (en) * | 2015-03-16 | 2015-07-08 | 吴江华诚复合材料科技有限公司 | Pressure-resistant ceramic material and preparation method thereof |
| CN105405651A (en) * | 2014-09-09 | 2016-03-16 | 株式会社村田制作所 | Multilayer Ceramic Capacitor |
-
2002
- 2002-11-08 CN CN 02151904 patent/CN1211316C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863221A (en) * | 2012-09-20 | 2013-01-09 | 广东风华高新科技股份有限公司 | Method, sintering aid and materials for preparation of low-temperature cofired medium ceramic and application |
| CN103295780A (en) * | 2013-06-20 | 2013-09-11 | 广东风华高新科技股份有限公司 | Manufacturing method for multi-layer ceramic capacitor |
| CN103295780B (en) * | 2013-06-20 | 2015-10-28 | 广东风华高新科技股份有限公司 | The preparation method of multilayer ceramic capacitor |
| CN103922714A (en) * | 2014-03-18 | 2014-07-16 | 福建火炬电子科技股份有限公司 | Low dielectric constant multi-layer capacitor ceramic material and preparation method thereof |
| CN103922714B (en) * | 2014-03-18 | 2015-09-16 | 福建火炬电子科技股份有限公司 | A kind of low-k multi-layer capacitor porcelain and preparation method thereof |
| CN105405651A (en) * | 2014-09-09 | 2016-03-16 | 株式会社村田制作所 | Multilayer Ceramic Capacitor |
| CN105405651B (en) * | 2014-09-09 | 2018-12-18 | 株式会社村田制作所 | Laminated ceramic capacitor |
| CN104761257A (en) * | 2015-03-16 | 2015-07-08 | 吴江华诚复合材料科技有限公司 | Pressure-resistant ceramic material and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1211316C (en) | 2005-07-20 |
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