CN116653380A - Ceramic material with layered structure - Google Patents
Ceramic material with layered structure Download PDFInfo
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- CN116653380A CN116653380A CN202310805732.7A CN202310805732A CN116653380A CN 116653380 A CN116653380 A CN 116653380A CN 202310805732 A CN202310805732 A CN 202310805732A CN 116653380 A CN116653380 A CN 116653380A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 68
- 239000000919 ceramic Substances 0.000 claims abstract description 75
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 22
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910001200 Ferrotitanium Inorganic materials 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 17
- 239000008139 complexing agent Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- 239000002985 plastic film Substances 0.000 claims description 5
- 229920006255 plastic film Polymers 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000010425 asbestos Substances 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- RIVZIMVWRDTIOQ-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co].[Co] RIVZIMVWRDTIOQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052895 riebeckite Inorganic materials 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 230000035939 shock Effects 0.000 abstract description 9
- 230000005621 ferroelectricity Effects 0.000 abstract description 8
- 230000005307 ferromagnetism Effects 0.000 abstract description 8
- 229910001429 cobalt ion Inorganic materials 0.000 abstract description 3
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 abstract description 3
- -1 iron ions Chemical class 0.000 abstract description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 abstract description 3
- 241001198704 Aurivillius Species 0.000 abstract description 2
- 239000011224 oxide ceramic Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 89
- 230000005291 magnetic effect Effects 0.000 description 19
- 239000010936 titanium Substances 0.000 description 16
- 239000000843 powder Substances 0.000 description 8
- 230000005684 electric field Effects 0.000 description 7
- 230000005415 magnetization Effects 0.000 description 7
- 230000005690 magnetoelectric effect Effects 0.000 description 7
- 230000010287 polarization Effects 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 5
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910000428 cobalt oxide Inorganic materials 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229910017135 Fe—O Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 238000009863 impact test Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 150000007514 bases Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 229920000642 polymer Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 150000002910 rare earth metals Chemical group 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/05—Interconnection of layers the layers not being connected over the whole surface, e.g. discontinuous connection or patterned connection
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/558—Impact strength, toughness
-
- 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
- C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a ceramic material with a layered structure, and belongs to the field of ceramic materials. Comprising a ceramic layer and an interface layer which are laminated. The invention combines the adjacent ceramic layers discontinuously through the interface layer, the high-speed impact energy forms compressive stress on the impacted surface of the ceramic, the invention combines the laminated ceramic structure with the weak interface (the weak combined interface is formed between the ceramic layers after co-sintering), can effectively separate and disperse the shock wave, prevent the damage caused by the concentrated shock wave, improve the quality protection capability, and the ceramic layer comprises the ferrotitanium bismuth cobaltate ceramic material, and replaces part of iron ions by cobalt ions to obtain Bi 7 Fe 3‑x Co x Ti 3 O 21 Layered Aurivillius type multiferroic oxideThe oxide ceramic can improve the ferroelectricity and ferromagnetism of ceramic materials. The data of the examples show that the ceramic material provided by the invention has both ferromagnetism and impact resistance.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a ceramic material with a layered structure.
Background
Magneto-electric effect is an important application of multiferroic materials. The magnetoelectric effect refers to the coupling effect among magnetic, mechanical force and electricity, namely, the magnetic field can change the electric polarization direction, the electric field can modulate the magnetization state, the multiferroic material with the magnetoelectric effect is paid attention to, and the magnetoelectric effect can be used for researching and developing ferroelectric and magnetic equipment, and can provide additional degrees of freedom for the design and application of the equipment due to the fact that the magnetoelectric effect can utilize the coupling between the magnetoelectric effect, so that the magnetoelectric effect has extremely attractive application prospect in emerging spintronics, polymorphic information storage, electrically driven ferromagnetic resonators and magnetically controlled piezoelectric sensors.
The magnetic ceramic is mainly ferrite ceramic, and ferrite is a composite oxide mainly composed of iron oxide and other iron group or rare earth group oxides. Ferrite belongs to semiconductor, has resistivity far greater than that of common metal magnetic material, and has the advantage of small eddy current loss. From the properties and applications of the magnetic ceramics, the magnetic ceramics can be classified into soft magnetic ceramics, hard magnetic ceramics, gyromagnetic ceramics, piezomagnetic bubbles, magneto-optical ceramics, thermosensitive ceramics and the like.
The magnetic ceramics in the prior art have the problem that ferromagnetism and impact resistance cannot be considered.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a ceramic material having a layered structure. The ceramic material prepared by the invention has both ferromagnetism and shock resistance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a ceramic material with a layered structure, which comprises ceramic layers and an interface layer, wherein the ceramic layers are arranged in a layered manner, the ceramic layers comprise a bismuth ferrocobaltate ceramic material, and the interface layer is made of a material capable of discontinuously combining adjacent ceramic layers.
Preferably, the chemical formula of the ferrotitanium bismuth cobaltate ceramic material is Bi 7 Fe 3-x Co x Ti 3 O 21 Wherein 0 is<x<3。
Preferably, the bismuth ferrotitanium cobaltate ceramic material is prepared by a method comprising the steps of:
mixing n-butyl titanate, a bismuth-containing compound, an iron-containing compound, a cobalt-containing compound and a complexing agent in acid liquor to obtain a mixed solution;
evaporating and presintering the mixed solution in sequence to obtain a precursor;
and sequentially tabletting, forming and sintering the precursor to obtain the ferrotitanium bismuth cobaltate ceramic material.
Preferably, the complexing agent is ethylenediamine tetraacetic acid and citric acid.
Preferably, the presintering temperature is 650-800 ℃ and the presintering time is 1-3 h.
Preferably, the sintering temperature is 870-890 ℃ and the sintering time is 1-10 h.
Preferably, the thickness of the ceramic layer is 1 to 15mm.
Preferably, the material of the interface layer includes one or more of paper sheets, plastic films, graphene, carbon nanotubes, carbon fibers, silicon carbide whiskers, alumina fibers, glass fibers, and asbestos.
Preferably, the thickness of the interface layer is 0.02-1 mm.
Preferably, the interfacial layer accounts for 10% -90% of the area of the ceramic layer.
The invention provides a ceramic material with a layered structure, which comprises ceramic layers and an interface layer, wherein the ceramic layers are arranged in a layered manner, the ceramic layers comprise a bismuth ferrocobaltate ceramic material, and the interface layer is made of a material capable of discontinuously combining adjacent ceramic layers.
Compared with the prior art, the invention has the following beneficial effects:
the ceramic material of the invention enables the adjacent ceramic layers to be discontinuously combined through the interface layer, the high-speed impact energy forms compressive stress on the impact surface of the ceramic, and the compressive stress is transferred to the reverse surface in the ceramic structure in the form of shock waves, and the ceramic material has the characteristics of high compressive strength but low tensile strength, so that the tensile stress formed by the shock waves damages the ceramic structure, thereby avoiding the adoption of uniform pressureThe ceramic material of the mass block body can completely transfer the energy of the impact wave until the back surface of the ceramic homogeneous block body, thereby causing the problem of integral crushing; the invention combines the laminated ceramic structure with weak interfaces (weak bonding interfaces are formed between ceramic layers after co-sintering), can effectively separate and disperse shock waves, prevent damage caused by concentrated shock waves, improve the quality protection capability, and the ceramic layer comprises ferrotitanium bismuth cobaltate ceramic material, and uses cobalt ions to replace part of iron ions to obtain Bi 7 Fe 3-x Co x Ti 3 O 21 Layered Aurivillius multiferroic oxide ceramic having a structure of two bismuth oxide layers ((Bi) 2 O 2 ) 2+ ) The titanium oxide (Ti-O) octahedron, the iron oxide (Fe-O) octahedron and the cobalt oxide (Co-O) octahedron are clamped between the two, wherein after partial cobalt ions replace partial iron ions, the arrangement of the Fe-O octahedron and the Co-O octahedron is relatively orderly, and the coupling between the Fe-O-Co can be locally generated, so that the ferroelectricity and ferromagnetism of the ceramic material can be improved. The data of the examples show that the ceramic material provided by the invention has both ferromagnetism and impact resistance.
Detailed Description
The invention provides a ceramic material with a layered structure, which comprises ceramic layers and an interface layer, wherein the ceramic layers are arranged in a layered manner, the ceramic layers comprise a bismuth ferrocobaltate ceramic material, and the interface layer is made of a material capable of discontinuously combining adjacent ceramic layers.
In the invention, the chemical formula of the ferrotitanium bismuth cobaltate ceramic material is preferably Bi 7 Fe 3-x Co x Ti 3 O 21 Wherein 0 is<x<3。
In the present invention, the x is preferably 0.5.ltoreq.x.ltoreq.2.
In the present invention, the bismuth ferrocobalt oxide ceramic material is preferably prepared by a method comprising the steps of:
mixing n-butyl titanate, a bismuth-containing compound, an iron-containing compound, a cobalt-containing compound and a complexing agent in acid liquor to obtain a mixed solution;
evaporating and presintering the mixed solution in sequence to obtain a precursor;
and sequentially tabletting, forming and sintering the precursor to obtain the ferrotitanium bismuth cobaltate ceramic material.
In the invention, the complexing agent is preferably ethylenediamine tetraacetic acid and citric acid, and the ethylenediamine tetraacetic acid (EDTA) and the citric acid can form a reticular polymer to stabilize metal ions on one hand, and can be used as a combustion improver in the subsequent sintering process on the other hand, so that the combustion heat production capacity is improved, and the preparation temperature of the ferrotitanium bismuth cobaltate ceramic material is further reduced. In addition, the invention takes ethylenediamine tetraacetic acid (EDTA) as a complexing agent, and avoids the reaction of excessive nitric acid and complexing agents such as glycol to generate oxalic acid, thereby avoiding the oxalic acid and metal ions from forming insoluble salts and precipitating out of the mixed solution. In the present invention, the mass ratio of the complexing agent to n-butyl titanate is preferably 25 to 45:5 to 10, more preferably 30 to 40:6 to 8. When complexing agents EDTA and citric acid, the mass ratio of EDTA, citric acid and n-butyl titanate is preferably 10-25:10-25:5-10, more preferably 15-20:10-20:6-8.
In the present invention, the temperature of the pre-firing is preferably 650 to 800 ℃, more preferably 680 to 770 ℃, most preferably 700 to 760 ℃, and the time is preferably 1 to 3 hours, more preferably 1.5 to 2.5 hours. In the invention, in the presintering process, the organic salt or the mixture of the organic salt and the metal acid salt in the powder generates strong oxidation-reduction reaction when being heated, and a large amount of gas is generated by combustion, so that the powder with high specific surface area is obtained, the reaction time is shortened, the reaction temperature is reduced, and the reaction efficiency is improved.
In the present invention, in order to prevent precipitation of metal ions from the mixed solution, the pH of the mixed solution is preferably adjusted to neutral before evaporating the mixed solution to dryness, that is, the mixed solution is adjusted to neutral with an alkaline compound. In the present invention, the basic compound is preferably aqueous ammonia.
In the present invention, the sintering temperature is preferably 870 to 890 ℃, and the time is preferably 1 to 10 hours.
In the invention, the n-butyl titanate provides a titanium source and can be chemically pure n-butyl titanate; the bismuth-containing compound provides a bismuth source and may be an analytically pure bismuth-containing compound, preferably one or more of bismuth nitrate pentahydrate, bismuth oxide and bismuth acetate, more preferably bismuth nitrate pentahydrate; the iron-containing compound provides a source of iron and may be an analytically pure iron-containing compound, preferably one or more of ferric nitrate nonahydrate, ferric oxide and ferric acetate, more preferably ferric nitrate nonahydrate; the cobalt-containing compound provides a cobalt source and may be an analytically pure cobalt-containing compound, preferably one or more of cobalt acetate tetrahydrate, cobalt oxide and cobalt nitrate hexahydrate, more preferably cobalt acetate tetrahydrate and/or cobalt nitrate hexahydrate, most preferably cobalt nitrate hexahydrate.
In the present invention, the thickness of the ceramic layer is preferably 1 to 15mm.
In the present invention, the material of the interface layer preferably includes one or more of paper sheets, plastic films, graphene, carbon nanotubes, carbon fibers, silicon carbide whiskers, alumina fibers, glass fibers, and asbestos.
In the present invention, the thickness of the interface layer is preferably 0.02 to 1mm.
In the present invention, the area ratio of the interface layer to the ceramic layer is preferably 10% to 90%, more preferably 70% to 80%, and the term "area ratio of the interface layer to the ceramic layer" means the area of the interface layer in contact with the ceramic layer. The contact area of the interface layer and the ceramic layer can be controlled to control the bonding strength of the upper ceramic layer and the lower ceramic layer after sintering.
In the invention, the ceramic material is formed by stacking a plurality of ceramic layers and interface layers and then co-sintering, and the ceramic material with a layered structure is prevented from being broken integrally by the layered structure design and the weak connection interface composition.
In the present invention, the ceramic material preferably has a multilayer structure in which two or more ceramic layers and interfacial layers between the ceramic layers are stacked, and the ceramic layers (the two or more ceramic layers) and the interfacial layers are alternately stacked, and the topmost layer and the bottommost layer of the multilayer structure are ceramic layers.
In the present invention, the interfacial layer hinders diffusion bonding of upper and lower ceramics during the co-sintering and is burned out to form voids during the ceramic sintering process, thereby forming weak bonding interfaces with voids on the overall structure, and at the same time, ceramic materials can be prepared at low cost.
The preparation method of the ceramic material with the layered structure is not particularly limited, and the preparation method can be performed by a mode well known to those skilled in the art, and specifically includes the following steps:
firstly, according to the required thickness, layer number, area ratio and the like, a multi-layer structure is formed by using corresponding ceramic layer materials and interface layer materials, wherein the ceramic layers and the interface layers are mutually staggered and laminated, and the topmost layer and the bottommost layer of the multi-layer structure are ceramic layers. According to the requirement of impact resistance (protection), a sheet ceramic blank with a certain thickness and a certain layer number can be designed and prepared, the ceramic blank is stacked, a compound interlayer or a paper sheet and a plastic film sheet material (film gap layer) are discontinuously paved between layers, and then the ceramic material is obtained by pressing and forming a multi-layer structure and then sintering. And sintering the stacked ceramic green bodies at a high temperature to form the layered ceramic armor which is integrally and completely combined and has discontinuous interfaces. The firing schedule is consistent with this type of ceramic firing schedule. Sintering can be performed in a general manner.
The ceramic material is prepared by combining the laminated ceramic structure with the weak interface, so that the shock waves can be effectively blocked and dispersed, damage caused by the concentrated shock waves is prevented, and the quality protection capability is improved; the layered structure can prevent the ceramic material from being damaged integrally, reduce the fragmentation area after the first striking and improve the striking resistance times of the ceramic material.
For further explanation of the present invention, the ceramic materials of layered structure provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
7.1475g of 98% pure n-butyl titanate, 24.0110g of 99% pure bismuth nitrate pentahydrate, 5.6849g of 98.5% pure ferric nitrate nonahydrate and 2.0684g of 99.5% pure cobalt nitrate hexahydrate are dissolved in a nitric acid solution, and 18.6157g of 98% pure ethylenediamine tetraacetic acid and 98% pure citric acid are added19.1227g as a complexing agent, and stirring to obtain a mixed solution. Placing the mixed solution in a crucible, evaporating to dryness until the mixed solution burns to obtain powder, presintering the obtained powder in a muffle furnace at 750 ℃ for 2 hours, and removing organic matters to obtain a precursor; preparing a cylindrical sample with the dimension phi of 12mm multiplied by 2mm from the precursor under the pressure of less than 10MPa, and sintering the cylindrical sample in a muffle furnace at 880 ℃ for 5 hours to obtain Bi 7 Fe 2 Co 1 Ti 3 O 21 Bi with ferroelectric property measuring instrument 7 Fe 2 Co 1 Ti 3 O 21 The ferroelectric property measurement shows that the ceramic material shows ferroelectricity at normal temperature, and the remnant polarization (2 Pr) is 25 muC/cm when the measured electric field is 190kV/cm 2 Coercive field (2 Ec) is 232kV/cm for Bi 7 Fe 2 Co 1 Ti 3 O 21 The magnetic properties were measured, and the result showed that the magnetic properties were exhibited at normal temperature, and the residual magnetization (2 Mr) was 2.1emu/g.
3 layers of Bi are prepared by extrusion under 5MPa through a semi-wet forming process 7 Fe 2 Co 1 Ti 3 O 21 A plastic pug blank; the thickness of the surface layer blank is 5mm, the thickness of the middle layer blank is 2.5mm, the thickness of the bottom layer blank is 5mm, 3 layers of ceramic blanks are stacked, perforated paper sheets are paved between the layers, the hole area accounts for about 30% of the total area of the paper sheets, the thickness is 0.2mm, and the interface layer accounts for 70% of the area ratio of the ceramic layers. The paper sheet size is smaller than the blank, and the blank is 5mm away from four sides of the blank after being paved. And (3) placing the stacked green bodies into a press for pressurizing at 5MPa, so that 3 layers of green bodies are attached, and pressing into a curved surface shape. And (3) putting the green body into kiln furniture, drying, debonding, and sintering for 10 hours at 2000 ℃, wherein the thickness of the ceramic material with the layered structure after sintering is 10mm.
The properties of the ceramic material with the layered structure obtained were tested according to the "method for testing impact resistance of ceramic wares" (Standard No. GB/T38494-2020), the flexural strength was 1028MPa, and the impact strength was 1.7J/cm 2 . The ferroelectric property of the ceramic material with the layered structure is measured, and the result shows that the ceramic material shows ferroelectricity at normal temperature, and the remnant polarization intensity (2 Pr) is 21 mu C/cm when the measured electric field is 190kV/cm 2 Coercive field (2 Ec) was 214kV/cm, proceedingThe magnetic properties were measured, and the result showed that the magnetic properties were ferromagnetic at ordinary temperature, and the residual magnetization (2 Mr) was 1.4emu/g.
Example 2
7.1475g of n-butyl titanate with the purity of 98%, 24.0110g of bismuth nitrate pentahydrate with the purity of 99%, 4.2637g of ferric nitrate nonahydrate with the purity of 98.5% and 3.1026g of cobalt nitrate hexahydrate with the purity of 99.5% are dissolved in a nitric acid solution, 18.6157g of ethylenediamine tetraacetic acid with the purity of 98% and 19.1227g of citric acid with the purity of 98% are added as complexing agents, and the mixed solution is obtained after stirring. Placing the mixed solution in a crucible, evaporating to dryness until the mixed solution burns to obtain powder, presintering the obtained powder in a muffle furnace at 750 ℃ for 2 hours, and removing organic matters to obtain a precursor; preparing a cylindrical sample with the dimension phi of 12mm multiplied by 2mm from the precursor under the pressure of less than 10MPa, and sintering the cylindrical sample in a muffle furnace at 880 ℃ for 5 hours to obtain Bi 7 Fe 2 Co 1 Ti 3 O 21 Bi with ferroelectric property measuring instrument 7 Fe 1.5 Co 1.5 Ti 3 O 21 The ferroelectric property measurement shows that the ceramic material shows ferroelectricity at normal temperature, and the remnant polarization (2 Pr) is 14 muC/cm when the measured electric field is 190kV/cm 2 Coercive field (2 Ec) of 204kV/cm for Bi 7 Fe 2 Co 1 Ti 3 O 21 The magnetic properties were measured, and the result showed that the magnetic properties were exhibited at normal temperature, and the residual magnetization (2 Mr) was 2.0emu/g.
5 layers of Bi are prepared by extrusion under 5MPa through a semi-wet forming process 7 Fe 1.5 Co 1.5 Ti 3 O 21 A plastic pug blank; 5 layers of green bodies are stacked, 50% of hole area and 0.1mm thick punching plastic film are paved between the layers, and the area ratio of the interface layer to the ceramic layer is 50%. And placing the stacked green bodies into kiln furniture, hot-pressing at 2150 ℃ for sintering for 18 hours under 30MPa, wherein the thickness of the sintered ceramic material with the layered structure is 8mm, and the ceramic material has a 5-layer structure.
The properties of the ceramic material of the layered structure obtained were tested according to the "method for impact test of ceramic articles" (Standard No. GB/T38494-2020), flexural strength was 1248MPa, impact strength was 2.1J/cm 2 . Ceramic material with laminated structureThe ferroelectric property of the material is measured, and the result shows that the material shows ferroelectricity at normal temperature, and the remnant polarization intensity (2 Pr) is 11 mu C/cm when the measured electric field is 190kV/cm 2 The coercive field (2 Ec) was 194kV/cm and magnetic properties were measured, which revealed that at ordinary temperature, it exhibited ferromagnetism, and the residual magnetization (2 Mr) was 1.2emu/g.
Example 3
7.1475g of n-butyl titanate with the purity of 98%, 24.0110g of bismuth nitrate pentahydrate with the purity of 99%, 2.8425g of ferric nitrate nonahydrate with the purity of 98.5% and 4.1368g of cobalt nitrate hexahydrate with the purity of 99.5% are dissolved in a nitric acid solution, 18.6157g of ethylenediamine tetraacetic acid with the purity of 98% and 19.1227g of citric acid with the purity of 98% are added as complexing agents, and the mixed solution is obtained after stirring. Placing the mixed solution in a crucible, evaporating to dryness until the mixed solution burns to obtain powder, presintering the obtained powder in a muffle furnace at 750 ℃ for 2 hours, and removing organic matters to obtain a precursor; preparing a cylindrical sample with the dimension phi of 12mm multiplied by 2mm from the precursor under the pressure of less than 10MPa, and sintering the cylindrical sample in a muffle furnace at 880 ℃ for 5 hours to obtain Bi 7 Fe 2 Co 1 Ti 3 O 21 Bi with ferroelectric property measuring instrument 7 Fe 1 Co 2 Ti 3 O 21 The ferroelectric property measurement shows that the ceramic material shows ferroelectricity at normal temperature, and the remnant polarization intensity (2 Pr) is 10 muC/cm when the measured electric field is 190kV/cm 2 Coercive field (2 Ec) of 236kV/cm for Bi 7 Fe 1 Co 2 Ti 3 O 21 The magnetic properties were measured, and the result showed that the magnetic properties were exhibited at normal temperature, and the residual magnetization (2 Mr) was 0.2emu/g.
3 layers of Bi are prepared by extrusion under 5MPa through a semi-wet forming process 7 Fe 1 Co 2 Ti 3 O 21 A plastic pug blank; the thickness of the surface layer blank is 5mm, the thickness of the middle layer blank is 2.5mm, the thickness of the bottom layer blank is 5mm, 3 layers of ceramic blanks are stacked, perforated paper sheets are paved between the layers, the hole area accounts for about 30% of the total area of the paper sheets, the thickness is 0.2mm, and the interface layer accounts for 70% of the area ratio of the ceramic layers. The paper sheet size is smaller than the blank, and the blank is 5mm away from four sides of the blank after being paved. Placing the stacked green bodies into a pressPressurizing by a machine, pressurizing by 5MPa, bonding the 3 layers of blanks, and pressing into a curved surface shape. And (3) putting the green body into kiln furniture, drying, debonding, and sintering for 10 hours at 2000 ℃, wherein the thickness of the ceramic material with the layered structure after sintering is 10mm.
The properties of the ceramic material of the layered structure obtained were tested according to the "method for impact test of ceramic articles" (Standard No.: GB/T38494-2020), flexural strength was 1013MPa, and impact strength was 1.6J/cm 2 . The ferroelectric property of the ceramic material with the layered structure is measured, and the result shows that the ceramic material shows ferroelectricity at normal temperature, and the remnant polarization intensity (2 Pr) is 7 mu C/cm when the measured electric field is 190kV/cm 2 The coercive field (2 Ec) was 217kV/cm, and magnetic properties were measured, which revealed that at ordinary temperature, it exhibited ferromagnetism, and the residual magnetization (2 Mr) was 0.14emu/g.
The foregoing is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A ceramic material of layered structure, comprising ceramic layers and interface layers, wherein the ceramic layers comprise bismuth ferrocobaltate ceramic material, and the interface layers are formed by discontinuously bonding adjacent ceramic layers.
2. The ceramic material of claim 1, wherein the bismuth ferrocobalt ceramic material has the formula Bi 7 Fe 3-x Co x Ti 3 O 21 Wherein 0 is<x<3。
3. Ceramic material according to claim 2, characterized in that the bismuth ferrocobalt ceramic material is produced by a method comprising the steps of:
mixing n-butyl titanate, a bismuth-containing compound, an iron-containing compound, a cobalt-containing compound and a complexing agent in acid liquor to obtain a mixed solution;
evaporating and presintering the mixed solution in sequence to obtain a precursor;
and sequentially tabletting, forming and sintering the precursor to obtain the ferrotitanium bismuth cobaltate ceramic material.
4. A ceramic material according to claim 3, wherein the complexing agent is ethylenediamine tetraacetic acid and citric acid.
5. A ceramic material according to claim 3, wherein the pre-firing temperature is 650-800 ℃ for 1-3 hours.
6. A ceramic material according to claim 3, wherein the sintering is carried out at a temperature of 870-890 ℃ for a time of 1-10 hours.
7. Ceramic material according to claim 1 or 2, characterized in that the thickness of the ceramic layer is 1-15 mm.
8. The ceramic material of claim 1, wherein the material of the interface layer comprises one or more of paper sheets, plastic films, graphene, carbon nanotubes, carbon fibers, silicon carbide whiskers, alumina fibers, glass fibers, and asbestos.
9. Ceramic material according to claim 1 or 8, characterized in that the thickness of the interface layer is 0.02-1 mm.
10. The ceramic material of claim 1, wherein the interfacial layer comprises 10% to 90% of the area of the ceramic layer.
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| CN102863211A (en) * | 2012-10-10 | 2013-01-09 | 中国科学技术大学 | Titanium-iron-gadolinium cobaltate-bismuth ceramic material in layer structure and preparation method of titanium-iron-gadolinium cobaltate-bismuth ceramic material |
| CN102942361A (en) * | 2012-10-10 | 2013-02-27 | 中国科学技术大学 | Ferrotitanium bismuth cobaltate ceramic material having layered structure and preparation method thereof |
| JP2018002556A (en) * | 2016-07-04 | 2018-01-11 | 三菱電機株式会社 | Ceramic composite, radome for missile, method for producing ceramic composite, and method for producing radome for missile |
| CN111620695A (en) * | 2020-05-21 | 2020-09-04 | 中国科学院上海硅酸盐研究所 | Ceramic material with layered structure |
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| CN102863211A (en) * | 2012-10-10 | 2013-01-09 | 中国科学技术大学 | Titanium-iron-gadolinium cobaltate-bismuth ceramic material in layer structure and preparation method of titanium-iron-gadolinium cobaltate-bismuth ceramic material |
| CN102942361A (en) * | 2012-10-10 | 2013-02-27 | 中国科学技术大学 | Ferrotitanium bismuth cobaltate ceramic material having layered structure and preparation method thereof |
| JP2018002556A (en) * | 2016-07-04 | 2018-01-11 | 三菱電機株式会社 | Ceramic composite, radome for missile, method for producing ceramic composite, and method for producing radome for missile |
| CN111620695A (en) * | 2020-05-21 | 2020-09-04 | 中国科学院上海硅酸盐研究所 | Ceramic material with layered structure |
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