CN113121226A - Optical dielectric ferroelectric ceramic material and preparation method and application thereof - Google Patents
Optical dielectric ferroelectric ceramic material and preparation method and application thereof Download PDFInfo
- Publication number
- CN113121226A CN113121226A CN202110481507.3A CN202110481507A CN113121226A CN 113121226 A CN113121226 A CN 113121226A CN 202110481507 A CN202110481507 A CN 202110481507A CN 113121226 A CN113121226 A CN 113121226A
- Authority
- CN
- China
- Prior art keywords
- nbo
- ceramic material
- ferroelectric ceramic
- optical dielectric
- optical
- 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
- 230000003287 optical effect Effects 0.000 title claims abstract description 167
- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 title claims abstract description 147
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 45
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims description 43
- 238000005245 sintering Methods 0.000 claims description 38
- 239000000919 ceramic Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 21
- 239000011812 mixed powder Substances 0.000 claims description 20
- 238000003825 pressing Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 7
- 239000003990 capacitor Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract 1
- 230000007704 transition Effects 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 101
- 239000010955 niobium Substances 0.000 description 78
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 45
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 45
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 26
- 229910052726 zirconium Inorganic materials 0.000 description 26
- 229910000019 calcium carbonate Inorganic materials 0.000 description 23
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 23
- 229910000027 potassium carbonate Inorganic materials 0.000 description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 22
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 16
- 238000001816 cooling Methods 0.000 description 14
- 238000010586 diagram Methods 0.000 description 14
- 239000011651 chromium Substances 0.000 description 12
- 239000011572 manganese Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- 238000001035 drying Methods 0.000 description 8
- 230000009471 action Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229910021543 Nickel dioxide Inorganic materials 0.000 description 5
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical group O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 5
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 229910002115 bismuth titanate Inorganic materials 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000003892 spreading Methods 0.000 description 4
- 230000007480 spreading Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910003334 KNbO3 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G7/00—Capacitors in which the capacitance is varied by non-mechanical means; Processes of their manufacture
- H01G7/06—Capacitors in which the capacitance is varied by non-mechanical means; Processes of their manufacture having a dielectric selected for the variation of its permittivity with applied voltage, i.e. ferroelectric capacitors
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3215—Barium oxides or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3241—Chromium oxides, chromates, or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3275—Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention belongs to the technical field of ceramic materials, and particularly relates to an optical dielectric ferroelectric ceramic material, and a preparation method and application thereof. The invention provides an optical dielectric ferroelectric ceramic material, which has a chemical general formula of (1-x) (K)0.5Na0.5)NbO3‑xA(MyNb1‑y)O3‑δX is 0.005 to 0.10, y is 0.01 to 0.5; a is one or more of AII group elements, and M is one or more of transition metal elements. The invention reduces (K) by introducing transition metal0.5Na0.5)NbO3The band gap of the material realizes the semi-conduction, so that the optical dielectric ferroelectric ceramic material has high optical dielectric tuning rate, the dielectric constant of the optical dielectric ferroelectric ceramic material is changed when being excited by light, and the optical-to-optical dielectric is realizedNon-contact regulation and control of the dielectric property of the ferroelectric ceramic material.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to an optical dielectric ferroelectric ceramic material, and a preparation method and application thereof.
Background
The dielectric property refers to that under the action of an external electric field, a non-conductive object, namely a dielectric medium, generates excessive charges with different signs at one end close to a charged body, and generates excessive charges with the same sign at the other end, and the property of accumulating and losing electrostatic energy under the action of the electric field is generally expressed by a dielectric constant and a dielectric loss. The illumination causes some dielectric change, such as sulfide, oxide semiconductor materials and filled tridymite type structures of Mott insulator BaCoSiO4The dielectric constant changes under illumination, and such materials are commonly referred to as photodielectric materials.
In some dielectric crystals, the structure of the unit cell causes the centers of positive and negative charges to be misaligned to generate an electric dipole moment, which generates electric polarization strength unequal to zero, so that the crystals have spontaneous polarization, and the direction of the electric dipole moment can be changed due to an external electric field, so that the crystals have the characteristic similar to ferromagnetism, and the property of the crystals is called ferroelectricity. Ferroelectric material refers to a class of materials having a ferroelectric effect.
Some ferroelectric materials have photo-dielectric properties, for example BaTiO was reported by Nature Photonics in 20183The dielectric constant of the single crystal after optical excitation is greatly reduced; in the same year, the incorporation of Ba (Ti) into 0.88BNT-0.12BT materials was reported0.5Ni0.5)O3–δThe components, doping and external field action generate carriers to realize semi-conduction, and a ferroelectric semiconductor is formed. Currently, ferroelectric materials with photo-dielectric properties, such as potassium sodium niobate (KNN) and sodium bismuth titanate (BNT) ceramics, have attracted extensive attention and research on physical properties such as ferroelectric, piezoelectric, pyroelectric, energy storage, and dielectric properties, but the dielectric tunability of potassium sodium niobate (KNN) and sodium bismuth titanate (BNT) ceramics is low when light is excited.
Disclosure of Invention
In view of the above, the present invention provides an optical dielectric ferroelectric ceramic material and a preparation method thereof, and the ceramic material provided by the present invention has ferroelectric properties, can realize non-contact control of optical on dielectric properties, and has high control capability.
In order to achieve the purpose of the invention, the invention provides the following technical scheme:
the invention provides an optical dielectric ferroelectric ceramic material, which has a chemical general formula of (1-x) (K)0.5Na0.5)NbO3-xA(MyNb1-y)O3-δX is 0.005 to 0.10, y is 0.01 to 0.5;
a is one or more of AII group elements, and M is one or more of transition metal elements.
Preferably, a comprises one or more of Ca, Ba and Sr.
Preferably, the M comprises one or more of Mn, Ni, Co, Mo, Fe and Cr.
Preferably, the chemical formula of the optical dielectric ferroelectric ceramic material is:
0.97(K0.5Na0.5)NbO3-0.03Ca(Ni0.5Nb0.5)O3-δ、
0.955(K0.5Na0.5)NbO3-0.045Ca(Ni0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Ni0.5Nb0.5)O3-δ、
0.925(K0.5Na0.5)NbO3-0.075Ca(Ni0.5Nb0.5)O3-δ、
0.91(K0.5Na0.5)NbO3-0.09Ca(Ni0.5Nb0.5)O3-δ、
0.995(K0.5Na0.5)NbO3-0.005Ca(Co0.5Nb0.5)O3-δ、
0.99(K0.5Na0.5)NbO3-0.01Ca(Co0.5Nb0.5)O3-δ、
0.985(K0.5Na0.5)NbO3-0.015Ca(Co0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Co0.5Nb0.5)O3-δ、
0.975(K0.5Na0.5)NbO3-0.025Ca(Co0.5Nb0.5)O3-δ、
0.99(K0.5Na0.5)NbO3-0.01Ca(Fe0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Fe0.5Nb0.5)O3-δ、
0.97(K0.5Na0.5)NbO3-0.03Ca(Fe0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Mo0.5Nb0.5)O3-δ、
0.96(K0.5Na0.5)NbO3-0.04Ca(Mo0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Mo0.5Nb0.5)O3-δ、
0.97(K0.5Na0.5)NbO3-0.03Ca(Cr0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Cr0.5Nb0.5)O3-δ、
0.91(K0.5Na0.5)NbO3-0.09Ca(Cr0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Mn0.5Nb0.5)O3-δ、
0.96(K0.5Na0.5)NbO3-0.04Ca(Mn0.5Nb0.5)O3-δor
0.94(K0.5Na0.5)NbO3-0.06Ca(Mn0.5Nb0.5)O3-δ。
The invention also provides a preparation method of the optical dielectric ferroelectric ceramic material in the technical scheme, which comprises the following steps:
mixing a K source, a Na source, a Nb source, an A source and an M source according to the stoichiometric ratio of the chemical general formula of the optical dielectric ferroelectric ceramic material, and then carrying out ball milling to obtain ceramic raw material mixed powder;
and sequentially granulating, pressing and sintering the ceramic raw material mixed powder to obtain the optical dielectric ferroelectric ceramic material.
Preferably, the ball milling comprises sequentially performing a first ball milling and a second ball milling;
the rotating speed of the first ball mill and the rotating speed of the second ball mill are respectively 350-450 rpm, and the time is respectively 12-24 h.
Preferably, the method further comprises the following steps of: pre-burning the ball milling material obtained by the first ball milling; the pre-sintering temperature is 850-950 ℃, and the time is 2-6 h.
Preferably, the pressing pressure is 150-200 MPa, and the pressure maintaining time is 30-60 s.
Preferably, the sintering temperature is 1100-1300 ℃, and the time is 2-8 h.
The invention also provides the application of the optical dielectric ferroelectric ceramic material in the technical scheme or the optical dielectric ferroelectric ceramic material obtained by the preparation method in the technical scheme as an optical modulation capacitor or an optical switch.
The invention provides an optical dielectric ferroelectric ceramic material, which has a chemical general formula of (1-x) (K)0.5Na0.5)NbO3-xA(MyNb1-y)O3-δX is 0.005 to 0.10, y is 0.01 to 0.5; a is one or more of AII group elements, and M is one or more of transition metal elements. In the present invention, (K)0.5Na0.5)NbO3A second component A (B) as a base materialyNb1-y)O3By passingReduced incorporation of transition metals (K)0.5Na0.5)NbO3Band gap of the material, ((K))0.5Na0.5)NbO3The material is converted from a good insulator to a semiconductor with weak conductivity to realize the semi-conduction, so that the optical dielectric ferroelectric ceramic material has high optical dielectric tuning rate, the dielectric constant of the optical dielectric ferroelectric ceramic material is changed when being excited by light, and the non-contact regulation and control of the dielectric property of the optical dielectric ferroelectric ceramic material by the light are realized.
The test results of the examples show that the optical band gap of the optical dielectric ferroelectric ceramic material provided by the invention is obviously reduced (the optical band gap is far lower than that of the pure KNN-based ceramic by 3 eV), which indicates that the optical dielectric ferroelectric ceramic material provided by the invention is semiconductive; the maximum tuning rate under 365nm ultraviolet light and 80Hz frequency is 29.5% -82.9%, and the optical dielectric adjusting performance is provided; the resistance ratio is high in a bright and dark state, and the photoresistance switching performance is good; has obvious ferroelectric property.
Drawings
FIG. 1 is an XRD pattern of the optical dielectric ferroelectric ceramic material obtained in examples 1 to 5;
FIG. 2 is a graph showing the determination of band gap (E) using the relationship between absorption data and Tauc formula for examples 1 and 3g) A drawing;
FIG. 3 is a graph showing the determination of band gap (E) using the relationship between absorption data and Tauc formula for examples 6 and 9g) A drawing;
FIG. 4 is a sample drawing of a wire for bonding of examples 1, 3, 6 and 9;
FIG. 5 is a graph of the capacitance tuning rate at different frequencies for examples 1, 3, 6 and 9 under the influence of UV 365 nm;
FIG. 6 is a graph showing the on-off resistance ratio of the light source of the optical dielectric ferroelectric ceramic material obtained in examples 1 to 5;
FIG. 7 is a graph showing the on/off resistance ratios of light sources of the optical dielectric ferroelectric ceramic materials obtained in examples 6 to 10;
FIG. 8 is a P-E loop diagram at 1Hz of the optical dielectric ferroelectric ceramic material obtained in example 1;
FIG. 9 is a P-E loop diagram at 1Hz of the optical dielectric ferroelectric ceramic material obtained in example 2;
FIG. 10 is a P-E loop diagram at 1Hz of the optical dielectric ferroelectric ceramic material obtained in example 3;
FIG. 11 is a P-E loop diagram at 1Hz of the optical dielectric ferroelectric ceramic material obtained in example 4;
FIG. 12 is a P-E loop diagram at 1Hz of the optical dielectric ferroelectric ceramic material obtained in example 5.
Detailed Description
The invention provides an optical dielectric ferroelectric ceramic material, which has a chemical general formula of (1-x) (K)0.5Na0.5)NbO3-xA(MyNb1-y)O3-δX is 0.005 to 0.10, y is 0.01 to 0.5;
a is one or more of AII group elements, and M is one or more of transition metal elements.
In the invention, the chemical general formula of the optical dielectric ferroelectric ceramic material is (1-x) (K)0.5Na0.5)NbO3-xA(MyNb1-y)O3-δ(ii) a x is 0.005-0.10, preferably 0.01-0.09, and more preferably 0.02-0.09; y is 0.01 to 0.5, preferably 0.05 to 0.5, and more preferably 0.1 to 0.5. In the present invention, δ in the chemical formula of the optical dielectric ferroelectric ceramic material is a value that ensures electrical neutrality of the optical dielectric ferroelectric ceramic material. In the invention, A is one or more of AII group elements; the a preferably comprises one or more of Ca, Ba and Sr. In the present invention, the valence of the AII group element preferably includes Ca2+、Ba2+And Sr2+One or more of (a).
In the present invention, M is one or more of transition metal elements; the M preferably comprises one or more of Mn, Ni, Co, Mo, Fe and Cr. In the present invention, the valence of the transition metal element preferably includes Mn2+、Mn4+、Ni2+、Ni3+、Co2+、Co4+、Mo6+、Fe2+、Fe3+、Cr2+And Cr4+One or more of (a).
In the present invention, the general chemical formula of the optical dielectric ferroelectric ceramic material is preferably:
0.97(K0.5Na0.5)NbO3-0.03Ca(Ni0.5Nb0.5)O3-δ、
0.955(K0.5Na0.5)NbO3-0.045Ca(Ni0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Ni0.5Nb0.5)O3-δ、
0.925(K0.5Na0.5)NbO3-0.075Ca(Ni0.5Nb0.5)O3-δ、
0.91(K0.5Na0.5)NbO3-0.09Ca(Ni0.5Nb0.5)O3-δ、
0.995(K0.5Na0.5)NbO3-0.005Ca(Co0.5Nb0.5)O3-δ、
0.99(K0.5Na0.5)NbO3-0.01Ca(Co0.5Nb0.5)O3-δ、
0.985(K0.5Na0.5)NbO3-0.015Ca(Co0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Co0.5Nb0.5)O3-δ、
0.975(K0.5Na0.5)NbO3-0.025Ca(Co0.5Nb0.5)O3-δ、
0.99(K0.5Na0.5)NbO3-0.01Ca(Fe0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Fe0.5Nb0.5)O3-δ、
0.97(K0.5Na0.5)NbO3-0.03Ca(Fe0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Mo0.5Nb0.5)O3-δ、
0.96(K0.5Na0.5)NbO3-0.04Ca(Mo0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Mo0.5Nb0.5)O3-δ、
0.97(K0.5Na0.5)NbO3-0.03Ca(Cr0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Cr0.5Nb0.5)O3-δ、
0.91(K0.5Na0.5)NbO3-0.09Ca(Cr0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Mn0.5Nb0.5)O3-δ、
0.96(K0.5Na0.5)NbO3-0.04Ca(Mn0.5Nb0.5)O3-δor
0.94(K0.5Na0.5)NbO3-0.06Ca(Mn0.5Nb0.5)O3-δ。
The invention also provides a preparation method of the optical dielectric ferroelectric ceramic material in the technical scheme, which comprises the following steps:
mixing a K source, a Na source, a Nb source, an A source and an M source according to the stoichiometric ratio of the chemical general formula of the optical dielectric ferroelectric ceramic material, and then carrying out ball milling to obtain ceramic raw material mixed powder;
and sequentially granulating, pressing and sintering the ceramic raw material mixed powder to obtain the optical dielectric ferroelectric ceramic material.
According to the stoichiometric ratio of the chemical general formula of the optical dielectric ferroelectric ceramic material, a K source, a Na source, a Nb source, an A source and an M source are mixed and then ball-milled to obtain ceramic raw material mixed powder.
In the invention, the purities of the K source, the Na source, the Nb source, the A source and the M source are preferably more than or equal to 99%. The sources of the K source, Na source, Nb source, A source and M source are not particularly limited in the present invention, and commercially available products known to those skilled in the art are used. In the invention, according to the elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, the K source is preferably potassium carbonate; the Na source is preferably sodium carbonate; the Nb source is preferably niobium pentoxide; the Ca source is preferably calcium carbonate; the Ba source is preferably barium carbonate; the Sr source is preferably strontium carbonate; the Mn source is preferably manganese dioxide; the Ni source is preferably nickel protoxide; the Co source is preferably cobaltous oxide; the Mo source is preferably molybdenum trioxide; the Fe source is preferably ferric oxide; the source of Cr is preferably chromium sesquioxide.
In the present invention, the ball milling preferably includes sequentially performing a first ball milling and a second ball milling.
In the invention, the rotating speed of the first ball mill is preferably 350-450 rpm, more preferably 370-430 rpm, and still more preferably 380-420 rpm; the time is preferably 12 to 24 hours, more preferably 14 to 22 hours, and still more preferably 16 to 20 hours. In the invention, the grinding balls in the first ball milling are preferably graded zirconium balls; the graded zirconium balls preferably comprise large zirconium balls and small zirconium balls; the diameter of the large zirconium ball is preferably 7-8 mm, and more preferably 7.2-7.8 mm; the diameter of the small zirconium balls is preferably 3-4 mm, and more preferably 3.2-3.8 mm; the diameter ratio of the large zirconium balls to the small zirconium balls is preferably (1.5-2.5): (0.5 to 1.5), most preferably 2: 1. in the invention, the number ratio of the large zirconium balls to the small zirconium balls is preferably (0.5-1.5): (1.5-2.5), most preferably 1: 2. in the invention, the ball-to-material ratio in the first ball milling is preferably (2-3): 1, more preferably (2.2 to 2.8): 1. in the present invention, the liquid medium in the first ball milling is preferably absolute ethanol. In the invention, the solid content of the slurry in the first ball milling is preferably 45-55%, and more preferably 47-53%. In the present invention, the first ball milling apparatus is preferably a tumbling ball mill. In the present invention, the particle size of the ball mill obtained after the first ball milling is preferably not more than 0.5 μm, and more preferably 0.2 to 0.3 μm. The invention improves the dispersion degree of the prepared materials through the first ball milling.
In the invention, the rotation speed of the second ball mill is preferably 350-450 rpm, more preferably 370-430 rpm, and still more preferably 380-420 rpm; the time is preferably 12 to 24 hours, more preferably 14 to 22 hours, and still more preferably 16 to 20 hours. In the invention, the grinding balls in the second ball milling are preferably graded zirconium balls; the graded zirconium balls preferably comprise large zirconium balls and small zirconium balls; the diameter of the large zirconium ball is preferably 7-8 mm, and more preferably 7.2-7.8 mm; the diameter of the small zirconium balls is preferably 3-4 mm, and more preferably 3.2-3.8 mm; the diameter ratio of the large zirconium balls to the small zirconium balls is preferably 2: 1. in the present invention, the number ratio of the large zirconium balls to the small zirconium balls is preferably 1: 2. in the invention, the ball-to-material ratio in the second ball milling is preferably (2-3): 1, more preferably (2.2 to 2.8): 1. in the present invention, the liquid medium in the second ball milling is preferably absolute ethanol. In the invention, the solid content of the slurry in the second ball milling is preferably 45-55%, and more preferably 47-53%. In the present invention, the second ball milling apparatus is preferably a tumbling ball mill. In the present invention, the particle size of the ceramic raw material mixed powder obtained after the second ball milling is preferably 0.03 to 0.08 μm, and more preferably 0.03 to 0.05 μm. The invention refines the grain diameter of the mixed powder of the ceramic raw materials by secondary ball milling.
In the present invention, it is preferable that the second ball mill further comprises, before the second ball milling: and pre-sintering the ball milling material obtained by the first ball milling. In the invention, the pre-sintering temperature is preferably 850-950 ℃, more preferably 860-940 ℃, and further preferably 870-930 ℃; the time is preferably 2 to 6 hours, more preferably 3 to 5 hours, and still more preferably 3.5 to 4.5 hours. In the present invention, the pre-firing temperature is preferably obtained by raising the temperature to room temperature; the heating rate is preferably 3-5 ℃/min, and more preferably 3.5-4.5 ℃/min. After the pre-sintering, the obtained pre-sintered powder is preferably cooled along with the furnace.
Between the first ball milling and the pre-sintering, the invention preferably also comprises drying and sieving the ball grinding material obtained by the first ball milling. In the invention, the drying temperature is preferably 60-80 ℃, and more preferably 65-75 ℃; the time is preferably 3 to 5 hours, and more preferably 3 to 4 hours. The liquid medium in the first ball milling is removed by drying. In the present invention, the mesh number of the screen is preferably 100 meshes.
After the second ball milling, the method preferably further comprises drying and sieving the ceramic raw material mixed powder obtained by the second ball milling. In the invention, the drying temperature is preferably 60-80 ℃, and more preferably 65-75 ℃; the time is preferably 3 to 5 hours, and more preferably 3.5 to 4.5 hours. The invention removes the liquid medium in the ceramic raw material mixed powder by drying. In the present invention, the mesh number of the screen is preferably 100 meshes.
After the mixed powder of the ceramic raw materials is obtained, the mixed powder of the ceramic raw materials is sequentially granulated, pressed and sintered to obtain the optical dielectric ferroelectric ceramic material.
In the present invention, no binder is added to the pellets to reduce voids and defects caused by the molding binder. The granulation method of the present invention is not particularly limited, and granulation known to those skilled in the art may be employed.
In the invention, the pressing pressure is preferably 150-200 MPa, more preferably 160-190 MPa, and still more preferably 170-180 MPa; the dwell time is preferably 30 to 60 seconds, more preferably 35 to 60 seconds, and still more preferably 40 to 60 seconds. In the present invention, the pressing is preferably dry press molding. In the present invention, the pressing is preferably performed in a mold. The mold of the present invention is not particularly limited, and a mold known in the art may be used. In an embodiment of the invention, the die is preferably a cylindrical die. The present invention is not particularly limited to the specific pressing operation, and a pressing operation known to those skilled in the art may be employed.
In the invention, the sintering temperature is preferably 1100-1300 ℃, more preferably 1150-1250 ℃, and further preferably 1150-1200 ℃; the time is preferably 2 to 8 hours, more preferably 3 to 7 hours, and further preferably 4 to 6 hours. In the present invention, the sintering temperature is preferably obtained by raising the temperature to room temperature; the heating rate is preferably 1 to 4 ℃/min, and more preferably 1.5 to 3.5 ℃/min. The invention controls the heating rate reaching the sintering temperature, is beneficial to reducing the porosity of a sintered product and improving the density of the finally obtained optical dielectric ferroelectric ceramic material.
In the present invention, the sintering preferably includes: placing the pressed tablet on a burning bearing plate with zirconia powder spread on the surface, spreading ceramic raw material mixed powder on the surface of the tablet, then adopting a small crucible to hold the tablet upside down, sealing with zirconia powder, then using a large crucible to hold the small crucible upside down, then heating from room temperature to sintering temperature, and preserving heat for sintering. In the present invention, the setter plate is preferably a zirconium plate. In the present invention, the particle size of the zirconia powder is preferably 0.03 to 0.12mm, and more preferably 0.05 to 0.10 mm. Before the zirconia powder is paved on a burning bearing plate, the zirconia powder is preferably roasted; the roasting temperature is preferably 1250-1350 ℃, and more preferably 1270-1330 ℃; the roasting time is preferably 1-4 hours, and more preferably 1.5-3 hours. In the invention, the spreading amount of the ceramic raw material mixed powder on the surface of the tabletting is based on completely covering the tabletting; the powder spreading thickness of the ceramic raw material mixed powder on the surface of the pressed sheet is preferably 0.5-2 mm, more preferably 0.8-1.5 mm, and most preferably 1 mm. The sintering method is favorable for creating a closed environment, increasing the concentration of element atmosphere in the sealed environment, reducing the volatilization of alkali metal, improving the heat preservation effect and being favorable for successfully preparing the ferroelectric semiconductor ceramic material.
In the present invention, the sintering preferably further comprises cooling. In the present invention, the cooling preferably includes first cooling and second cooling performed in this order. In the invention, the termination temperature of the first cooling is preferably 400-600 ℃, more preferably 420-580 ℃, and further preferably 450-550 ℃; the heat preservation time is preferably 2-4 h, and more preferably 2.5-3.5 h. In the present invention, the cooling rate from the sintering temperature to the termination temperature of the first cooling is preferably 1 to 2 ℃/min, and more preferably 1.2 to 1.8 ℃/min. In the present invention, the termination temperature of the second cooling is room temperature, and the cooling method is preferably furnace cooling. The invention prevents the problems of overlarge internal stress and increased defects of the optical dielectric ferroelectric ceramic material caused by the fact that the sintered product is cooled too fast by controlling the cooling rate.
The invention also provides the application of the optical dielectric ferroelectric ceramic material in the technical scheme or the optical dielectric ferroelectric ceramic material obtained by the preparation method in the technical scheme as an optical modulation capacitor or an optical switch. The present invention is not limited to the above applications, and the optical tunable capacitor or the optical switch may be made of an optical dielectric ferroelectric ceramic material known to those skilled in the art.
In order to further illustrate the present invention, the following examples are provided to describe an optical dielectric ferroelectric ceramic material, its preparation method and application in detail, but they should not be construed as limiting the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In the embodiment, the preparation raw materials are purchased from markets, and the purity is more than or equal to 99%; the chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.97 (K)0.5Na0.5)NbO3-0.03Ca(Ni0.5Nb0.5)O3-δ；
The preparation method comprises the following steps:
2.5753g of Na is added according to the stoichiometric ratio of the elements in the chemical formula of the optical dielectric ferroelectric ceramic material2CO30.3033g of CaCO33.3683g of K2CO30.1132g of NiO2And 13.1304g of Nb2O5Mixing and placing in a roller ball mill, taking zirconium balls with the diameters of 3.8mm and 7.6mm as grinding balls (the number ratio of the zirconium balls with the diameters of 3.8mm and 7.6mm is 2: 1), adding 80mL of absolute ethyl alcohol as a liquid medium, carrying out first ball milling for 18h under the condition of the rotation speed of 400rpm, separating the obtained ball milling material strainer, drying in an oven at 70 ℃ for 3h, sieving by a 100-mesh sieve, placing in a crucible, heating to 950 ℃ at the speed of 4 ℃/min, presintering at 950 ℃ for 3h, and cooling along with the furnace to obtain presintering powder;
putting the obtained pre-sintered powder into a roller ball mill, adding 40mL of absolute ethyl alcohol serving as a liquid medium into zirconium balls with the diameters of 3.8mm and 7.6mm serving as grinding balls (the number ratio of the zirconium balls with the diameters of 3.8mm to 7.6mm is 2: 1), performing secondary ball milling for 18h at the rotation speed of 400rpm, separating the obtained ball milling material strainer, drying in an oven at 70 ℃ for 3h, and sieving with a 100-mesh sieve to obtain ceramic raw material mixed powder;
without adding a binder, 0.4g of ceramic raw material mixed powder is placed in a cylindrical die with the radius of 12mm, and pressure is maintained for 60s under the pressure of 150MPa for dry pressing forming, so that a pressed sheet is obtained;
placing the pressed sheet on a zirconium plate paved with zirconia powder (the grain diameter of the zirconia powder is 70 mu m, and the pressed sheet is presintered at 1300 ℃ for 2h), spreading ceramic raw material mixed powder with the thickness of 1mm on the surface of the pressed sheet (the pressed sheet is completely covered by the ceramic raw material mixed powder), covering the pressed sheet with a small crucible, sealing with the zirconia powder, covering the small crucible with a large crucible, placing the small crucible in a muffle furnace, heating from room temperature to 1160 ℃ at the speed of 1 ℃/min, preserving heat for 5h, cooling to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2h, and cooling to room temperature along with the furnace to obtain the optical dielectric ferroelectric ceramic material.
Example 2
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.955 (K)0.5Na0.5)NbO3-0.045Ca(Ni0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、NiO2And Nb2O5And (3) obtaining the optical dielectric ferroelectric ceramic material by the same technical means as the example 1 for preparing the material.
Example 3
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.94 (K)0.5Na0.5)NbO3-0.06Ca(Ni0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、NiO2And Nb2O5And (3) obtaining the optical dielectric ferroelectric ceramic material by the same technical means as the example 1 for preparing the material.
Example 4
The chemical formula of the designed optical dielectric ferroelectric ceramic material is 0.925 (K)0.5Na0.5)NbO3-0.075Ca(Ni0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、NiO2And Nb2O5And (3) obtaining the optical dielectric ferroelectric ceramic material by the same technical means as the example 1 for preparing the material.
Example 5
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.91 (K)0.5Na0.5)NbO3-0.09Ca(Ni0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、NiO2And Nb2O5And (3) obtaining the optical dielectric ferroelectric ceramic material by the same technical means as the example 1 for preparing the material.
The phase structures of the optical dielectric ferroelectric ceramic materials obtained in examples 1 to 5 were analyzed, and the obtained XRD patterns (XRD patterns with 2 theta in the range of 20 to 80 degrees) are shown in FIG. 1. As can be seen from FIG. 1, the XRD pattern obtained was compared with KNbO3By comparing the standard maps (JCPDS card numbers 73-0299), the main phases of all the examples are perovskite structures, and no second phase exists; the results show that all examples can form good solid solutions, resulting in the desired phase.
Example 6
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.995 (K)0.5Na0.5)NbO3-0.005Ca(Co0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Co2O3And Nb2O5In order to prepare the material, the method comprises the following steps of,the sintering temperature is 1150 ℃, and the rest technical means are consistent with the embodiment 1, so as to obtain the optical dielectric ferroelectric ceramic material.
Example 7
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.99 (K)0.5Na0.5)NbO3-0.01Ca(Co0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Co2O3And Nb2O5The sintering temperature is 1150 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 8
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.985 (K)0.5Na0.5)NbO3-0.015Ca(Co0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Co2O3And Nb2O5The sintering temperature is 1150 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 9
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.98 (K)0.5Na0.5)NbO3-0.02Ca(Co0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Co2O3And Nb2O5The sintering temperature is 1150 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 10
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.975 (K)0.5Na0.5)NbO3-0.025Ca(Co0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Co2O3And Nb2O5The sintering temperature is 1150 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 11
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.99 (K)0.5Na0.5)NbO3-0.01Ca(Fe0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Fe2O3And Nb2O5The sintering temperature for preparing the material is 1180 ℃, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 12
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.98 (K)0.5Na0.5)NbO3-0.02Ca(Fe0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Fe2O3And Nb2O5The sintering temperature for preparing the material is 1180 ℃, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 13
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.97 (K)0.5Na0.5)NbO3-0.03Ca(Fe0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Fe2O3And Nb2O5The sintering temperature for preparing the material is 1180 ℃, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 14
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.98 (K)0.5Na0.5)NbO3-0.02Ca(Mo0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、MoO3And Nb2O5The sintering temperature is 1150 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 15
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.96 (K)0.5Na0.5)NbO3-0.04Ca(Mo0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、MoO3And Nb2O5The sintering temperature is 1150 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 16
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.94 (K)0.5Na0.5)NbO3-0.06Ca(Mo0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、MoO3And Nb2O5The sintering temperature is 1150 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 17
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.97 (K)0.5Na0.5)NbO3-0.03Ca(Cr0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Cr2O3And Nb2O5The sintering temperature is 1200 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 18
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.94 (K)0.5Na0.5)NbO3-0.06Ca(Cr0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Cr2O3And Nb2O5The sintering temperature is 1200 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 19
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.91 (K)0.5Na0.5)NbO3-0.09Ca(Cr0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、Cr2O3And Nb2O5The sintering temperature is 1200 ℃ for preparing the material, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 20
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.98 (K)0.5Na0.5)NbO3-0.02Ca(Mn0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、MnO2And Nb2O5The sintering temperature for preparing the material is 1180 ℃, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 21
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.96 (K)0.5Na0.5)NbO3-0.04Ca(Mn0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、MnO2And Nb2O5The sintering temperature for preparing the material is 1180 ℃, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Example 22
The chemical formula of the optical dielectric ferroelectric ceramic material is designed to be 0.94 (K)0.5Na0.5)NbO3-0.06Ca(Mn0.5Nb0.5)O3-δ；
According to the stoichiometric ratio of elements in the chemical general formula of the optical dielectric ferroelectric ceramic material, taking Na as2CO3、CaCO3、K2CO3、MnO2And Nb2O5The sintering temperature for preparing the material is 1180 ℃, and the other technical means are consistent with those of the embodiment 1, so that the optical dielectric ferroelectric ceramic material is obtained.
Performance testing
1. Polishing the optical dielectric ferroelectric ceramic material obtained in the embodiments 1 to 22 until both surfaces are smooth, measuring an absorption spectrum by an ultraviolet visible near infrared spectrophotometer, and obtaining the optical dielectric ferroelectric ceramic material obtained in the embodiments 1 to 22 by a Tauc formulaOptical bandgap of material examples 1 and 3 determine the bandgap (E) using the relationship between the absorption data and the Tauc formulag) Referring to FIG. 2, examples 6 and 9 determine the band gap (E) using the relationship between the absorption data and the Tauc formulag) See fig. 3. As can be seen from FIGS. 2 and 3, the optical band gap of the optical dielectric ferroelectric ceramic material provided by the present invention has a significantly reduced optical band gap, which is much lower than the optical band gap of 3eV of pure KNN-based ceramic, indicating that the optical dielectric ferroelectric ceramic material provided by the present invention has been semiconductive.
2. Polishing the optical dielectric ferroelectric ceramic materials obtained in the embodiments 1 to 22 to a thickness of 0.5mm, respectively obtaining optical dielectric ferroelectric ceramic sheets; two copper wires are welded on one surface of the obtained optical dielectric ferroelectric ceramic plate respectively, and a sample object diagram of the welding wires of examples 1, 3, 6 and 9 is shown in figure 4; and then connecting two wires of each welding wire sample to the positive electrode and the negative electrode of a precision impedance analyzer respectively, and testing the capacitance tuning rate under the action of ultraviolet light with the wavelength of 365nm under different frequencies (40 Hz-40 MHz). The capacitance tuning rate of the different frequencies of the examples 1, 3, 6 and 9 under the action of the ultraviolet 365nm is shown in fig. 5, and as can be seen from fig. 5, all the examples provided by the invention show the tuning rate under the optical excitation, wherein the tuning rate of 82.9% is obtained at 80Hz in the example 6, which shows that the optical dielectric ferroelectric ceramic material provided by the invention realizes the good regulation and control of the dielectric constant under the optical excitation.
The maximum tuning rates of the optical dielectric ferroelectric ceramic materials obtained in examples 1 to 22 under 365nm ultraviolet light and 80Hz frequency are shown in Table 1.
TABLE 1 maximum tuning rates of the obtained optical dielectric ferroelectric ceramic materials of examples 1 to 22 under 365nm ultraviolet light and 80Hz frequency
As can be seen from Table 1, the maximum tuning rate of the optical dielectric ferroelectric ceramic material provided by the invention is 29.5% -82.9% under 365nm ultraviolet light and 80Hz frequency. According to the dielectric constant formula, the tuning rate of the ceramic capacitor can reflect the tuning rate of the dielectric constant under the same test method, so that the dielectric constant changes under the action of incident light, namely the optical dielectric adjusting performance is obtained, therefore, light has an obvious adjusting effect on the dielectric constant of the optical dielectric ferroelectric ceramic material provided by the invention, namely the optical dielectric ferroelectric ceramic material provided by the invention has the optical dielectric performance.
3. The light source switch resistance ratios of the optical dielectric ferroelectric ceramic materials obtained in examples 1 to 10 were tested, and the test charts are shown in fig. 6 and 7, wherein fig. 6 is a diagram of the light source switch resistance ratios of the optical dielectric ferroelectric ceramic materials obtained in examples 1 to 5, and fig. 7 is a diagram of the light source switch resistance ratios of the optical dielectric ferroelectric ceramic materials obtained in examples 6 to 10. As can be seen from fig. 6 and 7, in examples 1 to 10, resistance ratios in different bright and dark states are obtained, wherein the resistance ratio in the bright and dark state in example 5 is as high as 109, which shows that the optical dielectric ferroelectric ceramic material obtained by the technical scheme provided by the present invention has good optical resistance switching performance.
4. The ferroelectric properties of the optical dielectric ferroelectric ceramic materials obtained in examples 1 to 5 are tested, and the P-E loop diagrams of the optical dielectric ferroelectric ceramic materials at 1Hz are shown in fig. 8 to 12, wherein fig. 8 is the P-E loop diagram of the optical dielectric ferroelectric ceramic materials obtained in example 1 at 1 Hz; FIG. 9 is a P-E loop diagram at 1Hz of the optical dielectric ferroelectric ceramic material obtained in example 2; FIG. 10 is a P-E loop diagram at 1Hz of the optical dielectric ferroelectric ceramic material obtained in example 3; FIG. 11 is a P-E loop diagram at 1Hz of the opto-dielectric ferroelectric ceramic material obtained in example 4; FIG. 12 is a P-E loop diagram at 1Hz of the optical dielectric ferroelectric ceramic material obtained in example 5. As can be seen from FIGS. 8 to 12, the optical dielectric ferroelectric ceramic materials provided in examples 1 to 5 all showed significant ferroelectric properties, which are shown by the following Ca (Ni)0.5Nb0.5)O3The content of constituent elements is increased and decreased, Pmax(maximum polarization) from 28.2. mu.C/cm2Down to 10.3. mu.C/cm2，Pr(remanent polarization) from 12.9. mu.C/cm2The concentration is reduced to 1.88 mu C/cm2At the same time, the P-E rings of examples 1 to 5 become elongated, and the photo-dielectric ferroelectric ceramic material was explainedThe relaxation performance of the material is gradually enhanced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The optical dielectric ferroelectric ceramic material is characterized in that the chemical general formula of the optical dielectric ferroelectric ceramic material is (1-x) (K)0.5Na0.5)NbO3-xA(MyNb1-y)O3-δX is 0.005 to 0.10, y is 0.01 to 0.5;
a is one or more of AII group elements, and M is one or more of transition metal elements.
2. The photodielectric ferroelectric ceramic material of claim 1, wherein a comprises one or more of Ca, Ba, and Sr.
3. The photodielectric ferroelectric ceramic material of claim 1, wherein M comprises one or more of Mn, Ni, Co, Mo, Fe, and Cr.
4. The photodielectric ferroelectric ceramic material of claim 1, having the chemical formula:
0.97(K0.5Na0.5)NbO3-0.03Ca(Ni0.5Nb0.5)O3-δ、
0.955(K0.5Na0.5)NbO3-0.045Ca(Ni0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Ni0.5Nb0.5)O3-δ、
0.925(K0.5Na0.5)NbO3-0.075Ca(Ni0.5Nb0.5)O3-δ、
0.91(K0.5Na0.5)NbO3-0.09Ca(Ni0.5Nb0.5)O3-δ、
0.995(K0.5Na0.5)NbO3-0.005Ca(Co0.5Nb0.5)O3-δ、
0.99(K0.5Na0.5)NbO3-0.01Ca(Co0.5Nb0.5)O3-δ、
0.985(K0.5Na0.5)NbO3-0.015Ca(Co0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Co0.5Nb0.5)O3-δ、
0.975(K0.5Na0.5)NbO3-0.025Ca(Co0.5Nb0.5)O3-δ、
0.99(K0.5Na0.5)NbO3-0.01Ca(Fe0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Fe0.5Nb0.5)O3-δ、
0.97(K0.5Na0.5)NbO3-0.03Ca(Fe0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Mo0.5Nb0.5)O3-δ、
0.96(K0.5Na0.5)NbO3-0.04Ca(Mo0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Mo0.5Nb0.5)O3-δ、
0.97(K0.5Na0.5)NbO3-0.03Ca(Cr0.5Nb0.5)O3-δ、
0.94(K0.5Na0.5)NbO3-0.06Ca(Cr0.5Nb0.5)O3-δ、
0.91(K0.5Na0.5)NbO3-0.09Ca(Cr0.5Nb0.5)O3-δ、
0.98(K0.5Na0.5)NbO3-0.02Ca(Mn0.5Nb0.5)O3-δ、
0.96(K0.5Na0.5)NbO3-0.04Ca(Mn0.5Nb0.5)O3-δor
0.94(K0.5Na0.5)NbO3-0.06Ca(Mn0.5Nb0.5)O3-δ。
5. A method for preparing an optical dielectric ferroelectric ceramic material as claimed in any one of claims 1 to 4, comprising the steps of:
mixing a K source, a Na source, a Nb source, an A source and an M source according to the stoichiometric ratio of the chemical general formula of the optical dielectric ferroelectric ceramic material, and then carrying out ball milling to obtain ceramic raw material mixed powder;
and sequentially granulating, pressing and sintering the ceramic raw material mixed powder to obtain the optical dielectric ferroelectric ceramic material.
6. The method of claim 5, wherein the ball milling comprises a first ball milling and a second ball milling in sequence;
the rotating speed of the first ball mill and the rotating speed of the second ball mill are respectively 350-450 rpm, and the time is respectively 12-24 h.
7. The preparation method according to claim 6, characterized by further comprising, before the second ball milling: pre-burning the ball milling material obtained by the first ball milling; the pre-sintering temperature is 850-950 ℃, and the time is 2-6 h.
8. The production method according to claim 5, wherein the pressure for the pressing is 150 to 200MPa, and the dwell time is 30 to 60 seconds.
9. The preparation method according to claim 5, wherein the sintering temperature is 1100-1300 ℃ and the sintering time is 2-8 h.
10. Use of the optical dielectric ferroelectric ceramic material according to any one of claims 1 to 4 or the optical dielectric ferroelectric ceramic material obtained by the preparation method according to any one of claims 5 to 9 as an optical tunable capacitor or an optical switch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110481507.3A CN113121226B (en) | 2021-04-30 | 2021-04-30 | Optical dielectric ferroelectric ceramic material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110481507.3A CN113121226B (en) | 2021-04-30 | 2021-04-30 | Optical dielectric ferroelectric ceramic material and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113121226A true CN113121226A (en) | 2021-07-16 |
| CN113121226B CN113121226B (en) | 2022-06-24 |
Family
ID=76780713
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110481507.3A Expired - Fee Related CN113121226B (en) | 2021-04-30 | 2021-04-30 | Optical dielectric ferroelectric ceramic material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113121226B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114057482A (en) * | 2021-11-30 | 2022-02-18 | 华中科技大学 | Sodium bismuth titanate-based ferroelectric ceramic gel-casting preparation method |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060286364A1 (en) * | 2005-06-15 | 2006-12-21 | Yueh-Ling Lee | Polymer-based capacitor composites capable of being light-activated and receiving direct metalization, and methods and compositions related thereto |
| JP2012069580A (en) * | 2010-09-21 | 2012-04-05 | Toyota Central R&D Labs Inc | Dielectric ceramic for tunable devices |
| CN104030683A (en) * | 2014-06-12 | 2014-09-10 | 中国人民解放军空军工程大学 | (K0.5Na0.5)NbO3-Sr(Sc0.5Nb0.5)O3 leadless transparent ferroelectric ceramic material and preparation method thereof |
| CN106588011A (en) * | 2016-12-31 | 2017-04-26 | 陕西师范大学 | Potassium sodium niobate-based leadless transparent ferroelectric ceramic with high remanent polarization and high Curie temperature, and production method thereof |
| CN106747669A (en) * | 2016-12-29 | 2017-05-31 | 陕西师范大学 | A kind of high-curie temperature and the good potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material of temperature stability and preparation method thereof |
| CN109485417A (en) * | 2018-11-19 | 2019-03-19 | 福州大学 | A kind of erbium/lanthanum relied on fluorescence temperature is co-doped with the preparation method of potassium-sodium niobate crystalline ceramics |
| CN110041074A (en) * | 2019-06-03 | 2019-07-23 | 桂林电子科技大学 | A kind of up-conversion luminescence transparent ferroelectric ceramics ceramic material and its preparation method and application |
| CN110372378A (en) * | 2019-07-22 | 2019-10-25 | 福州大学 | The potassium-sodium niobate photochromic transparent ceramics and preparation method thereof that europium/barium strontium titanate is modified altogether |
-
2021
- 2021-04-30 CN CN202110481507.3A patent/CN113121226B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060286364A1 (en) * | 2005-06-15 | 2006-12-21 | Yueh-Ling Lee | Polymer-based capacitor composites capable of being light-activated and receiving direct metalization, and methods and compositions related thereto |
| JP2012069580A (en) * | 2010-09-21 | 2012-04-05 | Toyota Central R&D Labs Inc | Dielectric ceramic for tunable devices |
| CN104030683A (en) * | 2014-06-12 | 2014-09-10 | 中国人民解放军空军工程大学 | (K0.5Na0.5)NbO3-Sr(Sc0.5Nb0.5)O3 leadless transparent ferroelectric ceramic material and preparation method thereof |
| CN106747669A (en) * | 2016-12-29 | 2017-05-31 | 陕西师范大学 | A kind of high-curie temperature and the good potassium-sodium niobate-based transparent ferroelectric ceramics ceramic material of temperature stability and preparation method thereof |
| CN106588011A (en) * | 2016-12-31 | 2017-04-26 | 陕西师范大学 | Potassium sodium niobate-based leadless transparent ferroelectric ceramic with high remanent polarization and high Curie temperature, and production method thereof |
| CN109485417A (en) * | 2018-11-19 | 2019-03-19 | 福州大学 | A kind of erbium/lanthanum relied on fluorescence temperature is co-doped with the preparation method of potassium-sodium niobate crystalline ceramics |
| CN110041074A (en) * | 2019-06-03 | 2019-07-23 | 桂林电子科技大学 | A kind of up-conversion luminescence transparent ferroelectric ceramics ceramic material and its preparation method and application |
| CN110372378A (en) * | 2019-07-22 | 2019-10-25 | 福州大学 | The potassium-sodium niobate photochromic transparent ceramics and preparation method thereof that europium/barium strontium titanate is modified altogether |
Non-Patent Citations (3)
| Title |
|---|
| JIE ZHANG等: "Photo-dielectric response enhancement and switching behavior of (1-x) (K0.5Na0.5)NbO3-xCa(Ni0.5Nb0.5)O3-δ ceramics by semiconduction method", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| YANG BAI等: "Multi-functional perovskites — an investigation of compositional and processing influence on microstructure, dielectric and ferroelectric properties", 《THE EUROPEAN PHYSICAL JOURNAL SPECIAL TOPICS》 * |
| 李彦德: "（1-x）（K0.5Na0.5）NbO3- xM(Fe0.5Nb0.5）O3(M=Ca、Sr)复合型钙钛矿之介电性质研究", 《成功大学材料科学与工程学系学位论文》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114057482A (en) * | 2021-11-30 | 2022-02-18 | 华中科技大学 | Sodium bismuth titanate-based ferroelectric ceramic gel-casting preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113121226B (en) | 2022-06-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109574656A (en) | A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material and preparation method thereof | |
| CN109133915A (en) | A kind of high energy storage barium phthalate base dielectric material and preparation method thereof | |
| CN109180178A (en) | A kind of barium-strontium titanate-based unleaded relaxation ferroelectric ceramic of high energy storage density and preparation method thereof | |
| CN109942292B (en) | Sodium bismuth titanate-based transparent ceramic material and preparation method and application thereof | |
| CN110436920B (en) | Sodium bismuth titanate-sodium tantalate solid-solution ceramic material and preparation method and application thereof | |
| CN111747740B (en) | Samarium ion doped lead zirconate titanate based high-performance piezoelectric ceramic and preparation method thereof | |
| CN110981476A (en) | Potassium sodium niobate-based transparent ceramic material and preparation method thereof | |
| CN106187181A (en) | A kind of based on PZT based antiferroelectric material rolling membrane process and preparation method thereof | |
| CN107140974A (en) | A kind of unleaded high energy storage density ST NBT ceramic materials of microwave sintering and preparation method thereof | |
| Truong-Tho et al. | Effect of sintering temperature on the dielectric, ferroelectric and energy storage properties of SnO2-doped Bi 0. 5 (Na 0. 8 K 0. 2) 0. 5 TiO3 lead-free ceramics | |
| CN109384465A (en) | A kind of preparation method of samarium doping potassium-sodium niobate crystalline ceramics | |
| CN113121226B (en) | Optical dielectric ferroelectric ceramic material and preparation method and application thereof | |
| CN107473732B (en) | Strontium titanate-based ceramic material with high energy storage density and low dielectric loss and preparation method thereof | |
| CN108863348A (en) | A kind of dielectric ceramic material and preparation method thereof of ultra-wide temperature stability | |
| CN107188554A (en) | A kind of preparation method of ceramic target | |
| CN111004030B (en) | MgTiO (magnesium-titanium-oxide) powder3Microwave-based dielectric ceramic and preparation method thereof | |
| CN112851346A (en) | Ultra-low-loss zirconium magnesium niobate system microwave dielectric ceramic material and preparation method thereof | |
| CN116425543A (en) | B-bit high-entropy ceramic with high energy storage and charge-discharge performance as dielectric material and preparation method thereof | |
| CN109650875B (en) | Giant dielectric calcium copper titanate composite ceramic material and preparation method and application thereof | |
| CN102976748A (en) | High-density barium strontium titanate ceramic and preparation method thereof | |
| CN114478006A (en) | KNNS-BNZ + CuO piezoceramic material and preparation method and application thereof | |
| CN114436643A (en) | Giant dielectric constant and low dielectric loss ceramic and preparation method thereof | |
| CN109320243A (en) | A kind of preparation method of the potassium-sodium niobate of the high grade of transparency-barium strontium crystalline ceramics | |
| CN104098330B (en) | Post growth annealing is adopted to prepare the method for high-performance barium strontium titanate pyroelectric ceramics | |
| CN116082034B (en) | Bismuth sodium titanate-based high-entropy ceramic material with high energy storage characteristic, and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20210716 Assignee: GUANGXI WUZHOU MICRO-MAGNET TECHNOLOGY Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2022450000243 Denomination of invention: A kind of optical dielectric ferroelectric ceramic material and its preparation method and application Granted publication date: 20220624 License type: Common License Record date: 20221206 |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20220624 |