CN110342924A - A kind of high-temperature ceramic capacitor dielectric material and preparation method thereof - Google Patents
A kind of high-temperature ceramic capacitor dielectric material and preparation method thereof Download PDFInfo
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- CN110342924A CN110342924A CN201910617297.9A CN201910617297A CN110342924A CN 110342924 A CN110342924 A CN 110342924A CN 201910617297 A CN201910617297 A CN 201910617297A CN 110342924 A CN110342924 A CN 110342924A
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 20
- 239000003989 dielectric material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002019 doping agent Substances 0.000 claims abstract description 27
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 229910002118 Bi2Ti2O7 Inorganic materials 0.000 claims abstract description 14
- 229910004774 CaSnO3 Inorganic materials 0.000 claims abstract description 14
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 14
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 14
- 229910021523 barium zirconate Inorganic materials 0.000 claims abstract description 14
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 14
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 14
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 14
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910017676 MgTiO3 Inorganic materials 0.000 claims abstract description 11
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 8
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 5
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000012265 solid product Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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Abstract
The present invention provides a kind of high-temperature ceramic capacitor dielectric material and preparation method thereof, it include: principal component and modifying dopant, the principal component and the quality proportioning of modifying dopant are principal component 80-90 parts, 10-20 parts of modifying dopant, and the principal component includes MgTiO3、Bi2Ti2O7、CeZr2O6、BaTiO3、BaZrO3、SrTiO3、CaSnO3、MgCO3、CuO、ZnO、Fe2O3、La2O3、Nb2O5、Sm2O3；The modifying dopant includes Al2O3、MnCO3、Y2O3、Dy2O3, preparation process of the present invention is simple, and material has the feature of environmental protection, while sintering temperature is lower, is conducive to energy saving.
Description
Technical field
The present invention relates to technical field of novel materials, specially a kind of high-temperature ceramic capacitor dielectric material and its preparation side
Method.
Background technique
In recent years, with the continuous development of electronic industry, currently on the market (especially phone charger etc.), to porcelain dielectric
The quality requirement of container is higher and higher, should minimize and also want high reliablity development & production high reliability and miniaturization porcelain dielectric
The container key technical problem to be solved is exactly to develop high performance ceramic capacitor dielectric material, and the country is corresponding at present
Material is gradually difficult to meet demand for development.Therefore exploitation has higher electric strength, and more low dielectric loss is wider to use temperature model
It encloses, the technology of preparing of the ceramic capacitor dielectric material of high reliablity, and realizes industrialization, be that current domestic electronics industry continues
One of emphasis of development.
Summary of the invention
Technical problem solved by the invention is to provide a kind of high-temperature ceramic capacitor dielectric material and preparation method thereof,
To solve the problems mentioned in the above background technology.
Technical problem solved by the invention is realized using following technical scheme: a kind of high-temperature ceramic capacitor medium material
Material, comprising: the quality proportioning of principal component and modifying dopant, the principal component and modifying dopant is principal component 80-90 parts, changes
10-20 parts of dopant of property, the principal component includes MgTiO3、Bi2Ti2O7、CeZr2O6、 BaTiO3、BaZrO3、SrTiO3、
CaSnO3、MgCO3、CuO、ZnO、Fe2O3、La2O3、Nb2O5、Sm2O3；Its quality proportioning is MgTiO35-10 parts, Bi2Ti2O710-
20 parts, CeZr2O65-10 parts, BaTiO310-20 parts, BaZrO35-10 parts, SrTiO35-10 parts, CaSnO31-5 parts, MgCO31-5
Part, CuO1-5 parts, ZnO1-5 parts, Fe2O31-5 parts, La2O31-5 parts, Nb2O51-5 parts, Sm2O31-5 parts.
Its quality proportioning of the principal component is MgTiO35 parts, Bi2Ti2O710 parts, CeZr2O65 parts, BaTiO310 parts,
BaZrO35 parts, SrTiO35 parts, CaSnO31 part, MgCO31 part, CuO1 parts, ZnO1 parts, Fe2O31 part, La2O31 part, Nb2O51
Part, Sm2O31 part.
Its quality proportioning of the principal component is MgTiO310 parts, Bi2Ti2O720 parts, CeZr2O610 parts, BaTiO320 parts,
BaZrO310 parts, SrTiO310 parts, CaSnO35 parts, MgCO35 parts, CuO5 parts, ZnO5 parts, Fe2O35 parts, La2O35 parts, Nb2O55
Part, Sm2O35 parts.
Its quality proportioning of the principal component is MgTiO38 parts, Bi2Ti2O715 parts, CeZr2O68 parts, BaTiO315 parts,
BaZrO38 parts, SrTiO38 parts, CaSnO33 parts, MgCO33 parts, CuO3 parts, ZnO3 parts, Fe2O33 parts, La2O33 parts, Nb2O53
Part, Sm2O33 parts.
The modifying dopant includes Al2O3、MnCO3、Y2O3、Dy2O3, quality proportioning Al2O310-20 parts,
MnCO310-20 parts, Y2O31-5 parts, Dy2O31-5 parts.
A kind of preparation method of high-temperature ceramic capacitor dielectric material, comprising the following steps:
Principal component is crushed to granularity in 200 mesh hereinafter, obtaining principal component powder by step 1.；
Principal component powder is put into ball milling 4 hours in planetary ball mill by step 2.；It is sub when the planetary ball mill ball milling
Ball milling is carried out under the atmosphere of nitrogen, Material quality of grinding balls is stainless steel, and ratio of grinding media to material example is 8:1, revolving speed 200r*min-1；
Step 3. using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Later under vacuum conditions
It is sintered using vacuum drying oven, after sintering, cools to room temperature with the furnace and obtain compound intermediate；
Modifying dopant is crushed to granularity in 200 mesh hereinafter, obtaining modifying dopant powder by step 4.；Then HCl is added
Modifying dopant is dissolved into solution by solution, later be added step 3 obtained in compound intermediate, and adjust its pH be 4.5~
5.0, the reaction was stirred for 2 to 6 hours, and the solid product in gained suspension is ceramic powders；
Step 5. by ceramic powders using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Exist later
It is sintered under vacuum condition using vacuum drying oven, is warming up to 600~650 DEG C and keeps the temperature 2~3 hours；Then heat to 1000~
It is sintered at 1200 DEG C, keeps the temperature 2~3 hours to get finished product ceramics.
It is 10 that vacuum drying oven sintering parameter, which is vacuum degree, in the step 4-2~10-1Pa, sintering temperature are 850~1000
DEG C, pressure is 20~35MPa, 5~10min of soaking time.
Heating rate is 4~5 DEG C/min in the step 3, step 5.
Compared with prior art, the beneficial effects of the present invention are: preparation process of the present invention is simple, and material has environmental protection
Property, while sintering temperature is lower, is conducive to energy saving.
Specific embodiment
In order to make implement technical means of the invention, creation characteristic, reach purpose and effect is easy to understand, further
Illustrate the present invention, in the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ",
" company ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or being integrally connected can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also indirectly connected through an intermediary, it can two
Connection inside a element.
Embodiment 1
A kind of preparation method of high-temperature ceramic capacitor dielectric material, comprising the following steps:
Quality proportioning is MgTiO by step 1.35 parts, Bi2Ti2O710 parts, CeZr2O65 parts, BaTiO310 parts, BaZrO35
Part, SrTiO35 parts, CaSnO31 part, MgCO31 part, CuO1 parts, ZnO1 parts, Fe2O31 part, La2O31 part, Nb2O51 part, Sm2O31
The principal component of part is crushed to granularity in 200 mesh hereinafter, obtaining principal component powder；
Principal component powder is put into ball milling 4 hours in planetary ball mill by step 2.；It is sub when the planetary ball mill ball milling
Ball milling is carried out under the atmosphere of nitrogen, Material quality of grinding balls is stainless steel, and ratio of grinding media to material example is 8:1, revolving speed 200r*min-1；
Step 3. using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Later under vacuum conditions
It is sintered using vacuum drying oven, after sintering, cools to room temperature with the furnace and obtain compound intermediate；
Quality proportioning is Al by step 4.2O310-20 parts, MnCO310-20 parts, Y2O31-5 parts, Dy2O31-5 parts of modification
Dopant is crushed to granularity in 200 mesh hereinafter, obtaining modifying dopant powder；Then HCl solution is added, modifying dopant is molten
Compound intermediate obtained in step 3 is added at solution in solution later, and adjusting its pH is 4.5~5.0, and it is small to be stirred to react 2~6
When, the solid product in gained suspension is ceramic powders；Vacuum drying oven sintering parameter is that vacuum degree is 10-2~10-1Pa is burnt
Junction temperature is 850~1000 DEG C, and pressure is 20~35MPa, 5~10min of soaking time；
Step 5. by ceramic powders using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Exist later
It is sintered under vacuum condition using vacuum drying oven, is warming up to 600~650 DEG C and keeps the temperature 2~3 hours；Then heat to 1000~
It is sintered at 1200 DEG C, keeps the temperature 2~3 hours to get finished product ceramics.
Embodiment 2
A kind of preparation method of high-temperature ceramic capacitor dielectric material, comprising the following steps:
Quality proportioning is MgTiO by step 1.310 parts, Bi2Ti2O720 parts, CeZr2O610 parts, BaTiO320 parts,
BaZrO310 parts, SrTiO310 parts, CaSnO35 parts, MgCO35 parts, CuO5 parts, ZnO5 parts, Fe2O35 parts, La2O35 parts, Nb2O55
Part, Sm2O35 parts of principal component is crushed to granularity in 200 mesh hereinafter, obtaining principal component powder；
Principal component powder is put into ball milling 4 hours in planetary ball mill by step 2.；It is sub when the planetary ball mill ball milling
Ball milling is carried out under the atmosphere of nitrogen, Material quality of grinding balls is stainless steel, and ratio of grinding media to material example is 8:1, revolving speed 200r*min-1；
Step 3. using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Later under vacuum conditions
It is sintered using vacuum drying oven, after sintering, cools to room temperature with the furnace and obtain compound intermediate；
Quality proportioning is Al by step 4.2O310-20 parts, MnCO310-20 parts, Y2O31-5 parts, Dy2O31-5 parts of modification
Dopant is crushed to granularity in 200 mesh hereinafter, obtaining modifying dopant powder；Then HCl solution is added, modifying dopant is molten
Compound intermediate obtained in step 3 is added at solution in solution later, and adjusting its pH is 4.5~5.0, and it is small to be stirred to react 2~6
When, the solid product in gained suspension is ceramic powders；Vacuum drying oven sintering parameter is that vacuum degree is 10-2~10-1Pa is burnt
Junction temperature is 850~1000 DEG C, and pressure is 20~35MPa, 5~10min of soaking time；
Step 5. by ceramic powders using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Exist later
It is sintered under vacuum condition using vacuum drying oven, is warming up to 600~650 DEG C and keeps the temperature 2~3 hours；Then heat to 1000~
It is sintered at 1200 DEG C, keeps the temperature 2~3 hours to get finished product ceramics.
Embodiment 3
A kind of preparation method of high-temperature ceramic capacitor dielectric material, comprising the following steps:
Quality proportioning is MgTiO by step 1.38 parts, Bi2Ti2O715 parts, CeZr2O68 parts, BaTiO315 parts, BaZrO38
Part, SrTiO38 parts, CaSnO33 parts, MgCO33 parts, CuO3 parts, ZnO3 parts, Fe2O33 parts, La2O33 parts, Nb2O53 parts, Sm2O33
The principal component of part is crushed to granularity in 200 mesh hereinafter, obtaining principal component powder；
Principal component powder is put into ball milling 4 hours in planetary ball mill by step 2.；It is sub when the planetary ball mill ball milling
Ball milling is carried out under the atmosphere of nitrogen, Material quality of grinding balls is stainless steel, and ratio of grinding media to material example is 8:1, revolving speed 200r*min-1；
Step 3. using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Later under vacuum conditions
It is sintered using vacuum drying oven, after sintering, cools to room temperature with the furnace and obtain compound intermediate；
Quality proportioning is Al by step 4.2O310-20 parts, MnCO310-20 parts, Y2O31-5 parts, Dy2O31-5 parts of modification
Dopant is crushed to granularity in 200 mesh hereinafter, obtaining modifying dopant powder；Then HCl solution is added, modifying dopant is molten
Compound intermediate obtained in step 3 is added at solution in solution later, and adjusting its pH is 4.5~5.0, and it is small to be stirred to react 2~6
When, the solid product in gained suspension is ceramic powders；Vacuum drying oven sintering parameter is that vacuum degree is 10-2~10-1Pa is burnt
Junction temperature is 850~1000 DEG C, and pressure is 20~35MPa, 5~10min of soaking time；
Step 5. by ceramic powders using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Exist later
It is sintered under vacuum condition using vacuum drying oven, is warming up to 600~650 DEG C and keeps the temperature 2~3 hours；Then heat to 1000~
It is sintered at 1200 DEG C, keeps the temperature 2~3 hours to get finished product ceramics.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.Claimed range of the invention by appended claims and
Its equivalent thereof.
Claims (8)
1. a kind of high-temperature ceramic capacitor dielectric material, it is characterised in that: include: principal component and modifying dopant, it is described it is main at
Divide and the quality proportioning of modifying dopant is principal component 80-90 parts, 10-20 parts of modifying dopant, the principal component includes
MgTiO3、Bi2Ti2O7、CeZr2O6、BaTiO3、BaZrO3、SrTiO3、CaSnO3、MgCO3、CuO、ZnO、Fe2O3、La2O3、
Nb2O5、Sm2O3；Its quality proportioning is MgTiO35-10 parts, Bi2Ti2O710-20 parts, CeZr2O65-10 parts, BaTiO310-20 parts,
BaZrO35-10 parts, SrTiO35-10 parts, CaSnO31-5 parts, MgCO31-5 parts, CuO1-5 parts, ZnO1-5 parts, Fe2O31-5 parts,
La2O31-5 parts, Nb2O51-5 parts, Sm2O31-5 parts.
2. a kind of high-temperature ceramic capacitor dielectric material according to claim 1, it is characterised in that: its matter of the principal component
Amount proportion is MgTiO35 parts, Bi2Ti2O710 parts, CeZr2O65 parts, BaTiO310 parts, BaZrO35 parts, SrTiO35 parts, CaSnO31
Part, MgCO31 part, CuO1 parts, ZnO1 parts, Fe2O31 part, La2O31 part, Nb2O51 part, Sm2O31 part.
3. a kind of high-temperature ceramic capacitor dielectric material according to claim 1, it is characterised in that: its matter of the principal component
Amount proportion is MgTiO310 parts, Bi2Ti2O720 parts, CeZr2O610 parts, BaTiO320 parts, BaZrO310 parts, SrTiO310 parts,
CaSnO35 parts, MgCO35 parts, CuO5 parts, ZnO5 parts, Fe2O35 parts, La2O35 parts, Nb2O55 parts, Sm2O35 parts.
4. a kind of high-temperature ceramic capacitor dielectric material according to claim 1, it is characterised in that: its matter of the principal component
Amount proportion is MgTiO38 parts, Bi2Ti2O715 parts, CeZr2O68 parts, BaTiO315 parts, BaZrO38 parts, SrTiO38 parts, CaSnO33
Part, MgCO33 parts, CuO3 parts, ZnO3 parts, Fe2O33 parts, La2O33 parts, Nb2O53 parts, Sm2O33 parts.
5. a kind of high-temperature ceramic capacitor dielectric material according to claim 1, it is characterised in that: the modifying dopant
Including Al2O3、MnCO3、Y2O3、Dy2O3, quality proportioning Al2O310-20 parts, MnCO310-20 parts, Y2O31-5 parts, Dy2O31-
5 parts.
6. a kind of preparation method of high-temperature ceramic capacitor dielectric material, comprising the following steps:
Principal component is crushed to granularity in 200 mesh hereinafter, obtaining principal component powder by step 1.；
Principal component powder is put into ball milling 4 hours in planetary ball mill by step 2.；Sub- nitrogen when the planetary ball mill ball milling
Atmosphere under carry out ball milling, Material quality of grinding balls is stainless steel, and ratio of grinding media to material example is 8:1, revolving speed 200r*min-1；
Step 3. using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；It utilizes under vacuum conditions later
Vacuum drying oven is sintered, and after sintering, is cooled to room temperature with the furnace and is obtained compound intermediate；
Modifying dopant is crushed to granularity in 200 mesh hereinafter, obtaining modifying dopant powder by step 4.；Then HCl solution is added,
Modifying dopant is dissolved into solution, compound intermediate obtained in step 3 is added later, and adjusting its pH is 4.5~5.0,
The reaction was stirred for 2 to 6 hours, and the solid product in gained suspension is ceramic powders；
Step 5. by ceramic powders using pressure testing machine carry out tabletting, pressure 500MPa, pressure maintaining 3 minutes；Later in vacuum
Under the conditions of be sintered using vacuum drying oven, be warming up to 600~650 DEG C keep the temperature 2~3 hours；Then heat to 1000~1200 DEG C
Lower sintering keeps the temperature 2~3 hours to get finished product ceramics.
7. a kind of preparation method of high-temperature ceramic capacitor dielectric material according to claim 6, it is characterised in that: described
It is 10 that vacuum drying oven sintering parameter, which is vacuum degree, in step 4-2~10-1Pa, sintering temperature be 850~1000 DEG C, pressure be 20~
35MPa, 5~10min of soaking time.
8. a kind of preparation method of high-temperature ceramic capacitor dielectric material according to claim 6, it is characterised in that: described
Heating rate is 4~5 DEG C/min in step 3, step 5.
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