CN103864415B - Barium titanate high dielectric ceramic of a kind of zinc doping and preparation method thereof - Google Patents
Barium titanate high dielectric ceramic of a kind of zinc doping and preparation method thereof Download PDFInfo
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- CN103864415B CN103864415B CN201410044022.8A CN201410044022A CN103864415B CN 103864415 B CN103864415 B CN 103864415B CN 201410044022 A CN201410044022 A CN 201410044022A CN 103864415 B CN103864415 B CN 103864415B
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- dielectric ceramic
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Abstract
Barium titanate high dielectric ceramic of a kind of zinc doping and preparation method thereof, the component general formula of described pottery is (BaTiO
3)
0.98(Zn
2snO
4)
0.02, concrete preparation process comprises: (1) BaTiO
3the preparation of powder, (2) SnO
2-Zn
2snO
4preparation, (3) of powder mix pressed compact and (4) forming materials.Barium titanate high dielectric ceramic prepared by the present invention has higher specific inductivity, lower dielectric loss and splendid temperature stability, relative permittivity ε all remains between 5000-5500, and fluctuation range is within 10%, dielectric loss, below 0.1%, is with a wide range of applications.
Description
Technical field
The present invention relates to the dielectric ceramic in function ceramics field, specifically the preparation method of the barium titanate high dielectric ceramic that a kind of tindioxide-zinc is composite mixed.
Background technology
Dielectric ceramic material is because of its stable chemical nature, be easy to the product being prepared into different shape, size and direction of polarization, the pottery with different qualities that modification obtains being applicable to different needs is obtained by doping and displacement, and cheap, be thus widely used.
Have higher specific inductivity with the ferroelectric ceramic(s) that barium titanate or barium phthalate base sosoloid are principal crystalline phase, be one of important electron ceramic material manufacturing ferroelectric ceramic capacitor in electron trade.When device shape is determined, the specific inductivity of material is higher, and the ratio capacitance of electrical condenser is larger; The electric capacity variation with temperature rate of electrical condenser is less, and the temperature stability of material is better, and higher electric capacity and good temperature stability weigh the major criterion of device performance.Because lead is a kind of element environment and human body to high risks, according to the enforcement of country about unleaded policy, the ceramic raw material of unleaded class more and more will inevitably be used at future electronic china industry.In the application aspect of reality, the laminated ceramic capacitor (MLCC) using ferroelectric ceramic(s) to manufacture requires that the device volume of manufacture is little, capacitance per unit volume amount large, environmental factors change is little on device performance impact.According to industry standard, the composition of raw materials manufacturing MLCC will meet X7R, X8R, Y5U or Y5V standard, namely requires that product will have higher specific inductivity and relative high temperature stability.
Summary of the invention
Technical problem to be solved by this invention is to provide barium titanate high dielectric ceramic of a kind of zinc doping and preparation method thereof, made its relative permittivity of high dielectric ceramic reaches more than 5000, and having good frequency stability, dielectric loss is below 0.001, and temperature stability is good.
The present invention is the technical scheme solving the problems of the technologies described above employing: a kind of barium titanate high dielectric ceramic of zinc doping, the component general formula of described pottery is (BaTiO
3)
1-x(Zn
2snO
4)
x, wherein, x=0.02.
A preparation method for the barium titanate high dielectric ceramic of zinc doping, the principal phase of described barium titanate high dielectric ceramic is BaTiO
3and Zn
2snO
4, its preparation method is:
(1) BaTiO
3the preparation of powder: by BaCO
3and TiO
2carry out proportioning according to the mol ratio of 1:1, then Wet blend-milling 10-15h, take out after wet-milling and dry; The mixed powder of drying is pressed into base substrate under the pressure of 5 ~ 10MPa; Again the base substrate pressed is put into retort furnace, at 1100 DEG C, keep 3h, then naturally cool to room temperature, obtain BaTiO
3powder, for subsequent use;
(2) SnO
2-Zn
2snO
4the preparation of powder: by SnO
2carry out proportioning with ZnO according to the mol ratio of 1:2, then Wet blend-milling 10-15h, take out after wet-milling and dry; The mixed powder of drying is pressed into base substrate under the pressure of 5 ~ 10MPa; Again the base substrate pressed is put into retort furnace, at 1000 DEG C, keep 2h, then naturally cool to room temperature, obtain SnO
2-Zn
2snO
4powder, for subsequent use;
(3) pressed compact is mixed: the BaTiO obtained by step (1)
3the SnO that powder and step (2) obtain
2-Zn
2snO
4powder carries out proportioning according to the mol ratio of 98:2, then Wet blend-milling 10-15h, takes out and dry after wet-milling; Afterwards, in the slip after oven dry, add the polyvinyl alcohol solution of its quality 6%, after stirring, under the pressure of 7-12MPa, be pressed into base substrate;
(4) forming materials: base substrate 650 DEG C at the binder removal process 120min obtained by step (3), then keeps 2h at 1260 DEG C, be then cooled to room temperature, namely complete preparation.
In described wet-milling process, adopt dehydrated alcohol as the abrasive of wet-milling, the mass concentration of dehydrated alcohol is 99%, and its add-on is treat wet-milling siccative quality 30-40%.
The base substrate of described step (1) and the middle compacting of step (2) is the disc-shaped structure of diameter 30mm.
In described step (3), the blank diameter of compacting is 15mm, and thickness is 1.2mm.
In described preparation process, the rotating speed of grinding machine is 120r/min, and the bake out temperature after wet-milling is 100 DEG C ~ 120 DEG C.
The mill ball adopted in described grinding machine is zirconia ball, and ZrO in zirconia ball
2mass percent be 80%.
Zirconia ball used is mixed by the zirconia ball of three kinds of different diameters, and its diameter is respectively 8.5mm, 4.5mm, 2.6mm, and the mass ratio of three kinds of diameter zirconium oxide balls is 4:3:4.
Described BaCO
3, TiO
2, SnO
2analytical reagent is with ZnO.
In described step (3), the mass concentration of polyvinyl alcohol solution is 10%.
Beneficial effect of the present invention:
1, the barium titanate high dielectric ceramic prepared by the present invention has higher specific inductivity, lower dielectric loss and splendid temperature stability, compared with the barium titanate based ceramic that ordinary method is obtained, in identical temperature range, during as 25 ~ 100 DEG C, the barium titanate based ceramic relative permittivity ε that ordinary method obtains is about 2500, and fluctuation range is generally more than 30%; And barium titanate high dielectric ceramic relative permittivity ε prepared by present method all remains between 5000-5500, and fluctuation range is within 10%.
2, present invention process is simple, stable, and preparation cycle is short, is conducive to realizing industrialized mass.The high dielectric ceramic electrical condenser of preparation, be applicable to higher operating frequency, dielectric loss, below 0.1%, has clear superiority, and application prospect is very wide, possesses certain potential using value and economic worth, is conducive to the microminiaturization of electronic devices and components.
accompanying drawing illustrates:
The X-ray diffractogram of the high dielectric ceramic of Fig. 1 obtained by the present invention;
Fig. 2 is that doping ratio is the sample (i.e. the present invention obtain pottery) of 2% and the temperature of pure barium titanate and relative permittivity graph of a relation under 100Hz condition;
Fig. 3 is that doping ratio is the sample (i.e. the present invention obtain pottery) of 2% and the temperature of pure barium titanate and dielectric loss graph of a relation under 100Hz condition;
The high dielectric ceramic of Fig. 4 obtained by the present invention is 10 in frequency
2under the condition of Hz, temperature and relative permittivity graph of a relation;
The high dielectric ceramic of Fig. 5 obtained by the present invention is 10 in frequency
2.5under the condition of Hz, temperature and relative permittivity graph of a relation;
The high dielectric ceramic of Fig. 6 obtained by the present invention is 10 in frequency
3under the condition of Hz, temperature and relative permittivity graph of a relation;
The high dielectric ceramic of Fig. 7 obtained by the present invention is 10 in frequency
3.5under the condition of Hz, temperature and relative permittivity graph of a relation;
The high dielectric ceramic of Fig. 8 obtained by the present invention is 10 in frequency
4under the condition of Hz, temperature and relative permittivity graph of a relation;
The high dielectric ceramic of Fig. 9 obtained by the present invention is 10 in frequency
4.5under the condition of Hz, temperature and relative permittivity graph of a relation;
The high dielectric ceramic of Figure 10 obtained by the present invention is 10 in frequency
5under the condition of Hz, temperature and relative permittivity graph of a relation;
The high dielectric ceramic of Figure 11 obtained by this present invention is 10 in frequency
5.5under the condition of Hz, temperature and relative permittivity graph of a relation.
Embodiment
Following embodiment is only described in further detail the present invention, but does not form any limitation of the invention.
A barium titanate high dielectric ceramic for zinc doping, the component general formula of described pottery is (BaTiO
3)
1-x(Zn
2snO
4)
x, wherein, x=0.02.
A preparation method for the barium titanate high dielectric ceramic of zinc doping, comprises following two large steps:
First, BaTiO is prepared
3powder and SnO
2-Zn
2snO
4powder;
Secondly, by BaTiO
3and Zn
2snO
4powder, according to general formula (BaTiO
3)
0.98(Zn
2snO
4)
0.02carry out mixed in molar ratio, prepare barium titanate-based lead-free high dielectric ceramic under certain condition, the component of gained sample is as shown in Fig. 1 X ray diffracting spectrum.
Concrete operation method is as follows:
A preparation method for the barium titanate high dielectric ceramic of zinc doping, the principal phase of barium titanate high dielectric ceramic is BaTiO
3and Zn
2snO
4, its concrete steps are:
(1) BaTiO
3the preparation of powder: by BaCO
3and TiO
2carry out proportioning according to the mol ratio of 1:1, then Wet blend-milling 10-15h, take out after wet-milling and dry; The mixed powder of drying is pressed into base substrate under the pressure of 5 ~ 10MPa; Again the base substrate pressed is put into retort furnace, at 1100 DEG C, keep 3h, then naturally cool to room temperature, obtain BaTiO
3powder, for subsequent use;
(2) SnO
2-Zn
2snO
4the preparation of powder: by SnO
2carry out proportioning with ZnO according to the mol ratio of 1:2, then Wet blend-milling 10-15h, take out after wet-milling and dry; The mixed powder of drying is pressed into base substrate under the pressure of 5 ~ 10MPa; Again the base substrate pressed is put into retort furnace, at 1000 DEG C, keep 2h, then naturally cool to room temperature, obtain SnO
2-Zn
2snO
4powder, for subsequent use;
(3) pressed compact is mixed: the BaTiO obtained by step (1)
3the SnO that powder and step (2) obtain
2-Zn
2snO
4powder carries out proportioning according to the mol ratio of 98:2, then Wet blend-milling 10-15h, takes out and dry after wet-milling; Afterwards, in the slip after oven dry, add the polyvinyl alcohol solution of its quality 6%, after stirring, under the pressure of 7-12MPa, be pressed into base substrate;
(4) forming materials: base substrate 650 DEG C at the binder removal process 120min obtained by step (3), then keeps 2h at 1260 DEG C, be then cooled to room temperature, namely complete preparation.
In described wet-milling process, adopt dehydrated alcohol as the solvent of wet-milling, the mass concentration of dehydrated alcohol is 99%, and its add-on is 30-40% of mixed powder quality.
The base substrate of described step (1) and the middle compacting of step (2) is the disc-shaped structure of diameter 30mm.
In described step (3), the blank diameter of compacting is 15mm, and thickness is 1.2mm.
In described preparation process, the rotating speed of grinding machine is 120r/min, and the bake out temperature after wet-milling is 100 DEG C ~ 120 DEG C.
The mill ball adopted in described grinding machine is zirconia ball, and ZrO in zirconia ball
2mass percent be 80%.
Zirconia ball used is mixed by the zirconia ball of three kinds of different diameters, and its diameter is respectively 8.5mm, 4.5mm, 2.6mm, and the mass ratio of three kinds of diameter zirconium oxide balls is 4:3:4.
Described barium carbonate, titanium dioxide, tindioxide and zinc oxide are analytical reagent.
In described step (3), the mass concentration of polyvinyl alcohol solution is 10%.
Embodiment one
Analytical pure chemical reagent barium carbonate, titanium dioxide are dry mixed as BaTiO
3first wife expects, the barium carbonate of add-on according to 0.49mol of raw material and the titanium dioxide of 0.49mol, and mol ratio is 1:1; By BaTiO
3first wife expects to load in nylon ball grinder, and carry out ball milling after adding alcohol, rotating speed is 120 revs/min, and ball milling 12 hours, obtains slip; Then, after the slip after ball milling being dried at room temperature ~ 120 DEG C, send in powder compressing machine, under the condition of 7MPa, be pressed into the disk that diameter is 30 millimeters, disk is sent in retort furnace again, at 1100 DEG C, sinter 3 hours, then naturally cool to room temperature, utilize solid reaction process to obtain BaTiO
3powder, for subsequent use;
Analytical pure chemical reagent tindioxide, zinc oxide are dry mixed as SnO
2-Zn
2snO
4first wife expects, the tindioxide of add-on according to 0.00667mol of raw material and the zinc oxide of 0.01333mol, and mol ratio is 1:2; By SnO
2-Zn
2snO
4first wife expects to load in nylon ball grinder, and carry out ball milling after adding alcohol, rotating speed is 120 revs/min, and ball milling 12 hours, obtains slip; Then after the slip after ball milling being dried at room temperature ~ 120 DEG C, in feeding powder compressing machine, under the condition of 7MPa, be pressed into the disk that diameter is 30 millimeters, disk is sent in retort furnace again, within 2 hours, then naturally cool to room temperature at 1000 DEG C of sintering, prepare SnO
2-Zn
2snO
4powder, for subsequent use;
Respectively to the BaTiO in step 1
3snO in powder and step 2
2-Zn
2snO
4powder carries out pulverizing, grinding, then by two kinds of powders stoichiometrically for 98:2 carries out mixing and sending into ball mill, add alcohol and carry out ball milling, rotating speed is 120 revs/min, ball milling 12 hours, weighs its weight after being dried by the compound after ball milling at room temperature ~ 120 DEG C, then add its weight 6% in slip after the drying, concentration is the polyvinyl alcohol solution of 10%, send into powder compressing machine, under 9MPa condition, be pressed into diameter 15 millimeters, the disk of thick 1.2 millimeters;
The disk that step 3 is obtained binder removal 120 minutes under 650 DEG C of conditions, then 1260 DEG C of sintering 2 hours, cooling room temperature, obtains sample; Dielectric properties test is carried out to sample.
In above-mentioned steps, the alcohol added during ball milling, its concentration is 99%, and add-on the material 0.5cm not treating ball milling;
In above-mentioned steps, mill ball used during ball milling is zirconia ball, and the mass ratio of zirconia ball is 4:1, and the zirconia ball put into has three kinds, and its diameter is respectively: 8.5mm, 4.5mm, 2.6mm, and mass ratio is 4:3:4.
In sum, adopt two-step approach of the present invention, by synthesis, there is Formula B aTiO
3powder and SnO
2-Zn
2snO
4powder, then by BaTiO
3and Zn
2snO
4powder, according to general formula (BaTiO
3)
0.98(Zn
2snO
4)
0.02carry out mixed in molar ratio and be sintered to barium titanate based dielectric pottery, gained sample permittivity is temperature 25-100 DEG C, and frequency is 10
2~ 10
5.5within the scope of during Hz, as shown in Figure 3, specific inductivity is higher than more than 5000, and dielectric loss is below 0.1%, and temperature stability is less than 10%.The BaTiO prepared with existing method
3sill performance is compared, and has at workspace specific inductivity high, and temperature-stable performance waits clear superiority well, and dielectric loss is little also smaller, and application prospect is very wide, possesses certain potential using value and economic worth.
Claims (9)
1. a barium titanate high dielectric ceramic for zinc doping, is characterized in that: the component general formula of described pottery is (BaTiO
3)
1-x(Zn
2snO
4)
x, wherein, x=0.02;
The principal phase of the barium titanate high dielectric ceramic of described zinc doping is BaTiO
3and Zn
2snO
4, its concrete preparation method comprises the following steps:
(1) BaTiO
3the preparation of powder: by BaCO
3and TiO
2carry out proportioning according to the mol ratio of 1:1, then Wet blend-milling 10-15h, take out after wet-milling and dry; The mixed powder of drying is pressed into base substrate under the pressure of 5 ~ 10MPa; Again the base substrate pressed is put into retort furnace, at 1100 DEG C, keep 3h, then naturally cool to room temperature, obtain BaTiO
3powder, for subsequent use;
(2) SnO
2-Zn
2snO
4the preparation of powder: by SnO
2carry out proportioning with ZnO according to the mol ratio of 1:2, then Wet blend-milling 10-15h, take out after wet-milling and dry; The mixed powder of drying is pressed into base substrate under the pressure of 5 ~ 10MPa; Again the base substrate pressed is put into retort furnace, at 1000 DEG C, keep 2h, then naturally cool to room temperature, obtain SnO
2-Zn
2snO
4powder, for subsequent use;
(3) pressed compact is mixed: the BaTiO obtained by step (1)
3the SnO that powder and step (2) obtain
2-Zn
2snO
4powder carries out proportioning according to the mol ratio of 98:2, then Wet blend-milling 10-15h, takes out and dry after wet-milling; Afterwards, in the slip after oven dry, add the polyvinyl alcohol solution of its quality 6%, after stirring, under the pressure of 7-12MPa, be pressed into base substrate;
(4) forming materials: base substrate 650 DEG C at the binder removal process 120min obtained by step (3), then keeps 2h at 1260 DEG C, be then cooled to room temperature, namely complete preparation.
2. the barium titanate high dielectric ceramic of a kind of zinc doping according to claim 1, it is characterized in that: in described wet-milling process, adopt dehydrated alcohol as the abrasive of wet-milling, the mass concentration of dehydrated alcohol is 99%, and its add-on is treat wet-milling siccative quality 30-40%.
3. the barium titanate high dielectric ceramic of a kind of zinc doping according to claim 1, is characterized in that: the base substrate of described step (1) and the middle compacting of step (2) is the disc-shaped structure of diameter 30mm.
4. the barium titanate high dielectric ceramic of a kind of zinc doping according to claim 1, it is characterized in that: in described step (3), the blank diameter of compacting is 15mm, and thickness is 1.2mm.
5. the barium titanate high dielectric ceramic of a kind of zinc doping according to claim 1, it is characterized in that: in described preparation process, the rotating speed of grinding machine is 120r/min, and the bake out temperature after wet-milling is 100 DEG C ~ 120 DEG C.
6. the barium titanate high dielectric ceramic of a kind of zinc doping according to claim 1, is characterized in that: the mill ball adopted in described grinding machine is zirconia ball, and ZrO in zirconia ball
2mass percent be 80%.
7. the barium titanate high dielectric ceramic of a kind of zinc doping according to claim 6, it is characterized in that: zirconia ball used is mixed by the zirconia ball of three kinds of different diameters, its diameter is respectively 8.5mm, 4.5mm, 2.6mm, and the mass ratio of three kinds of diameter zirconium oxide balls is 4:3:4.
8. the barium titanate high dielectric ceramic of a kind of zinc doping according to claim 1, is characterized in that: described BaCO
3, TiO
2, SnO
2analytical reagent is with ZnO.
9. the barium titanate high dielectric ceramic of a kind of zinc doping according to claim 1, is characterized in that: in described step (3), the mass concentration of polyvinyl alcohol solution is 10%.
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| CN110590358A (en) * | 2019-10-11 | 2019-12-20 | 河南科技大学 | Strontium titanate-based dielectric ceramic with high energy storage density and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1389432A (en) * | 2001-06-01 | 2003-01-08 | 天津大学 | Dielectrical for multilayer microwave ceramic capacitor and its prepn. |
| CN1532166A (en) * | 2003-03-21 | 2004-09-29 | 广东风华高新科技集团有限公司 | Method for producing high dielectric constant ceramic powder and ceramic capacitor |
| CN102584218A (en) * | 2012-02-14 | 2012-07-18 | 郴州功田电子陶瓷技术有限公司 | Environment-friendly microwave dielectric ceramic for L wave band |
-
2014
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1389432A (en) * | 2001-06-01 | 2003-01-08 | 天津大学 | Dielectrical for multilayer microwave ceramic capacitor and its prepn. |
| CN1532166A (en) * | 2003-03-21 | 2004-09-29 | 广东风华高新科技集团有限公司 | Method for producing high dielectric constant ceramic powder and ceramic capacitor |
| CN102584218A (en) * | 2012-02-14 | 2012-07-18 | 郴州功田电子陶瓷技术有限公司 | Environment-friendly microwave dielectric ceramic for L wave band |
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