CN106045500A - Preparation method of NBT-based high-temperature low-loss ceramic capacitor - Google Patents

Preparation method of NBT-based high-temperature low-loss ceramic capacitor Download PDF

Info

Publication number
CN106045500A
CN106045500A CN201610370589.3A CN201610370589A CN106045500A CN 106045500 A CN106045500 A CN 106045500A CN 201610370589 A CN201610370589 A CN 201610370589A CN 106045500 A CN106045500 A CN 106045500A
Authority
CN
China
Prior art keywords
ceramic capacitor
preparation
nbt
temperature low
tio
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.)
Pending
Application number
CN201610370589.3A
Other languages
Chinese (zh)
Inventor
蒲永平
万晶
吴煜蓉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201610370589.3A priority Critical patent/CN106045500A/en
Publication of CN106045500A publication Critical patent/CN106045500A/en
Pending legal-status Critical Current

Links

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
    • C04B35/475—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 based on bismuth titanates
    • 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
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
    • 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
    • C04B2235/3215—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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention discloses a preparation method of an NBT-based high-temperature low-loss ceramic capacitor. The chemical formula of the NBT-based high-temperature low-loss ceramic capacitor satisfies 0.92Na0.5Bi0.5TiO3-0.08BaTiO3-xLiBa2Nb5O15, wherein x represents mole fraction, and 0.2</=x</=0.5. The preparation method is characterized by including respectively preparing the main material Na0.5Bi0.5TiO3 and auxiliary materials BaTiO3 and LiBa2Nb5O15 through a solid phase method, sequentially performing blending, ball milling, drying and sieving according to proportion, then pressing to obtain a green body, performing heat preservation on the green body for 2-3 hours at 1120-1150 DEG C, sintering, and performing infiltration sintering to prepare electrodes so as to obtain the ceramic capacitor. The ceramic capacitor prepared by the method has the advantages that the ceramic capacitor uses NBT as the base body, a small amount of BaTiO3 is added into the base body, LiBa2Nb5O15 is doped for modification, and the doped LiBa2Nb5O15 can favorably lower the dielectric peak of the NBT to allow the NBT to keep low dielectric loss in a wide temperature range while the dielectric constant is relatively high.

Description

A kind of preparation method of NBT base high-temperature low-loss ceramic capacitor
[technical field]
The present invention relates to function ceramics field, particularly to the preparation of a kind of NBT base high-temperature low-loss ceramic capacitor Method.
[background technology]
In recent years, along with market demands improve constantly, the operating environment requirements residing for electronic equipment is harsher, example If the field such as Aero-Space, oil drilling operating ambient temperature is far above normal operating temperatures.But, along with the liter of operating temperature Height, the loss of electronic equipment is also increased dramatically, and is used for efficiency and creates the biggest impact.So, application temperature to the greatest extent may be used High low-loss multilayer ceramic capacitor can be kept to be particularly important simultaneously.
At present, leaded materials application is relatively broad, but owing to leaded oxide is unfavorable, to ring to the health of human body Border seriously polluted, so for environmental protection, exploitation lead-free ceramic capacitance device is necessary.For capacitor, ferroelectricity is situated between Matter has big dielectric constant values can meet the big requirement of capacitance, also adapts to the requirement of electronic equipment miniaturization simultaneously.But, greatly Dielectric constant makes dielectric loss the most correspondingly increase, so it is ceramic capacitor that unleaded and high-temperature scope has low-loss Two important development directions.
BaTiO3Pottery is owing to having good ferroelectric properties, piezoelectric property and higher dielectric constant, so being commonly used to Prepare multilayer ceramic capacitor.At present, most of high-temperature scopes have low-loss ceramic capacitor and are still with BaTiO3For Matrix, adulterating wherein, some compound modified achieve the goal.The high-temperature low-loss material being modified for matrix with NBT Material rarely has report.
[summary of the invention]
It is an object of the invention to overcome problems of the prior art, it is provided that a kind of NBT base high-temperature low-loss pottery The preparation method of porcelain condenser, with NBT as matrix, has relatively low-loss within the scope of high temperature.
For achieving the above object, the present invention adopts the following technical scheme that:
There are following steps:
(1) it is 0.92Na according to stoichiometric proportion0.5Bi0.5TiO3-0.08BaTiO3-xLiBa2Nb5O15, take BaTiO3Powder Body, Na0.5Bi0.5TiO3Powder body and LiBa2Nb5O15Powder body mixes, the mixture obtained is carried out ball milling, drying, pelletize and After sieving, forming screening material, wherein x represents molar fraction, 0.2≤x≤0.5；
(2) step (1) gained screening material is made sample, sample is burnt 1120～1150 DEG C of insulations for 2～3 hours Knot, is then cooled to room temperature；
(3), after the sample that polishing cleaning step (2) sinter, silver electrode paste is uniformly coated at sample tow sides, Sinter 30～40 minutes in 600～650 DEG C, obtain NBT base high-temperature low-loss ceramic capacitor.
Further, BaTiO3The preparation process of powder body includes: is first according to mol ratio 1:1 and weighs BaCO3And TiO2Formed Mixture A, taking mixture A with zirconium ballstone and deionized water is 1:(1～2 according to mass ratio): 1 mixing and ball milling 3～4h, and 60 ～80 DEG C of drying, then at 1120～1150 DEG C of calcinings, prepare BaTiO3Powder body.
Further, Na0.5Bi0.5TiO3The preparation process of powder body includes: is first according to mol ratio 1:1:4 and weighs Na2CO3、 Bi2O3And TiO2Forming mixture B, taking mixture B and zirconium ballstone and deionized water is 1:(1～2 according to mass ratio): 1 mixes ball Mill 3～4h, and 60～80 DEG C of drying, then at 800～850 DEG C of calcinings, prepare Na0.5Bi0.5TiO3Powder body.
Further, LiBa2Nb5O15The preparation process of powder body includes: is first according to mol ratio 4:1:5 and weighs BaCO3, Li2CO3And Nb2O5Forming mixture C, taking mixture C and zirconium ballstone and deionized water is 1:(1～2 according to mass ratio): 1 mixes Ball milling 3～4h 60～80 DEG C of drying, then at 1000～1100 DEG C of calcinings, prepares LiBa2Nb5O15Powder body.
Further, x=0.2,0.3,0.4 or 0.5.
Further, the drying temperature in step (1) is 60～80 DEG C.
Further, in step (1), formed after mixture, zirconium ballstone and deionized water mixing, ball milling, drying and dry material, By mass concentration be 5～6% binding agent add to dry material in carry out pelletize, obtain granulation material, binding agent account for drying material matter The 9～10% of amount.
Further, sieving in step (1) is that granulation material 40 mesh and 80 mesh sieves excessively respectively are taken middle material, it is thus achieved that screening Material；In step (2), screening material makes sample under the pressure of 110～120MPa.
Further, in step (2), sample first carries out binder removal process and is sintered, and it is 600 by sample that binder removal processes ～the Muffle furnace of 700 DEG C is incubated 30～40min.
Further, in step (2), sample is placed in the aluminium oxide saggar with zirconium oxide as backing plate at high temperature box furnace In, be warming up to 500 DEG C with 2 DEG C/min, then with 5 DEG C/min be warming up to 1120～1150 DEG C be incubated 2～3 hours, finally with 5 DEG C/ After min is cooled to 500 DEG C, cool to room temperature with the furnace.
Compared with prior art, the present invention has a following useful technique effect:
1. the present invention uses solid phase method to prepare, technical maturity, is suitable for industrialization and produces.2., with NBT as matrix, add wherein Enter a small amount of BaTiO3, main employing has the LiBa of ultra-low loss2Nb5O15It is doped modification, LiBa2Nb5O15Incorporation favourable In the dielectric peak forcing down NBT so that it is in the case of dielectric constant of a relatively high (＞ 1500), simultaneously can be at 70～402 DEG C Within the temperature range of, relatively low dielectric loss (≤2%) can be kept；3. learnt by contrast, LiBa2Nb5O15Interpolation permissible It is significantly expanded the loss temperature range less than 0.02, makes pottery keep ultralow dielectric to damage within the scope of the highest wider temperature Consumption, and chemical composition of the present invention and preparation technology are simple, cheaper starting materials environmental protection, the NBT base high temperature that therefore prepared by the inventive method Degree low-loss ceramic capacitor, has broad application prospects, and has the pottery of ultra-low loss under high-temperature for research further Porcelain condenser is laid a good foundation.
[accompanying drawing explanation]
Fig. 1 is the dielectric loss variation with temperature curve chart of embodiment of the present invention 1-4.
Fig. 2 is to be not added with LiBa in pottery2Nb5O15Dielectric loss vary with temperature figure.
[detailed description of the invention]
The present invention comprises the steps:
(1) BaTiO is first prepared3、Na0.5Bi0.5TiO3、LiBa2Nb5O15Standby:
1. BaCO is weighed according to mol ratio 1:13And TiO2Form mixture A；Take mixture A and zirconium ballstone and deionized water, According to mass ratio 1:(1～2): 1, mixing and ball milling 3～4h 60～80 DEG C of drying, then at 1120～1150 DEG C of calcining 3h, system Obtain powder body BaTiO3；
2. Na is weighed according to mol ratio 1:1:42CO3、Bi2O3And TiO2Form mixture B；Take mixture B and zirconium ballstone and Deionized water, according to mass ratio 1:(1～2): 1, mixing and ball milling 3～4h 60～80 DEG C of drying, forge then at 800～850 DEG C Burn 3h, prepare powder body Na0.5Bi0.5TiO3；
3. BaCO is weighed according to mol ratio 4:1:53, Li2CO3And Nb2O5Form mixture C；Take mixture C and zirconium ballstone and Deionized water, according to mass ratio 1:(1～2): 1, mixing and ball milling 3～4h 60～80 DEG C of drying, then at 1000～1100 DEG C Calcining 3h, prepares powder body LiBa2Nb5O15；
(2) the powder body BaTiO that step (1) is obtained3、Na0.5Bi0.5TiO3And LiBa2Nb5O15According to 0.92Na0.5Bi0.5TiO3-0.08BaTiO3-xLiBa2Nb5O15Dispensing, wherein x represents molar fraction, 0.2≤x≤0.5, takes mixed Compound and zirconium ballstone and deionized water, according to mass ratio 1:(1～2): 1, mixing and ball milling 3～4h, 60～80 DEG C is formed after drying Dry material, using mass concentration be 5～6% polyvinyl alcohol (PVA) add to drying in material as binding agent and to carry out pelletize, and point Not crossing 40 mesh and 80 mesh sieves take middle material, obtain screening material, wherein binding agent accounts for and dries the 9～10% of material quality；
(3) step (2) gained screening material is made ceramic green sample, first in Muffle under the pressure of 110～120MPa Binder removal in stove, binder removal be processed as in the Muffle furnace of 600～700 DEG C, be incubated ceramic green 30～40min with venting moisture and Organic substance, then, is placed in the aluminium oxide saggar with zirconium oxide as backing plate in high temperature box furnace, is warming up to 500 with 2 DEG C/min DEG C, it is warming up to 1120～1150 DEG C with 5 DEG C/min and is incubated 2～3 hours, then, after being cooled to 500 DEG C with 5 DEG C/min, cold with stove But to room temperature；
(4), after the sample that polishing, cleaning step (3) sinter, silver electrode paste is uniformly coated at sample tow sides, in 600～650 DEG C sinter 30～40 minutes, obtain NBT base high-temperature low-loss ceramic capacitor.
Embodiment 1:
NBT base high-temperature low-loss ceramic capacitor of the present invention, its formula is 0.92Na0.5Bi0.5TiO3-0.08BaTiO3- xLiBa2Nb5O15, wherein x=0.2, x represent molar fraction.
(1) BaTiO is prepared3、Na0.5Bi0.5TiO3、LiBa2Nb5O15Standby: to weigh BaCO according to mol ratio 1:13And TiO2 Form mixture A；Na is weighed according to mol ratio 1:1:42CO3、Bi2O3And TiO2Form mixture B；Claim according to mol ratio 4:1:5 Take BaCO3, Li2CO3And Nb2O5Form mixture C；
(2) taking mixture A, B, C, respectively with zirconium ballstone and deionized water, according to mass ratio 1:1:1, mixing and ball milling 4h is also 60 DEG C of drying, A in 1000 DEG C of calcinings, prepares powder body BaTiO in 850 DEG C of calcinings, C in 1150 DEG C of calcinings, B respectively3、 Na0.5Bi0.5TiO3、LiBa2Nb5O15；
(3) the powder body BaTiO that step (2) is obtained3、Na0.5Bi0.5TiO3And LiBa2Nb5O15According to 0.92Na0.5Bi0.5TiO3-0.08BaTiO3-xLiBa2Nb5O15Dispensing, wherein x=0.2, take mixture and deionized water, according to Mass ratio 1:1:1, mixing and ball milling 4h, 60 DEG C of drying, pelletizes, sieves, and forms granulation material；Wherein dry in material and add mass concentration Be 5% polyvinyl alcohol carry out pelletize, polyvinyl alcohol account for dry material quality 9%；
(4) step (3) gained granulation material is made under the pressure of 120MPa sample, first protect in the Muffle furnace of 600 DEG C Temperature 40min binder removal, then, is placed in the aluminium oxide saggar with zirconium oxide as backing plate in high temperature box furnace, heats up with 2 DEG C/min To 500 DEG C, it is warming up to 1120 DEG C with 5 DEG C/min and is incubated 2 hours, then, after being cooled to 500 DEG C with 5 DEG C/min, cool to the furnace Room temperature；
(5), after the sample that polishing, cleaning step (4) sinter, silver electrode paste is uniformly coated at sample tow sides, in 600 DEG C sinter 30 minutes, obtain NBT base high-temperature low-loss ceramic capacitor.
Embodiment 2
Only changing the molar fraction in formula into x=0.3, other condition is same as in Example 1.
Embodiment 3
Only changing the molar fraction in formula into x=0.4, other condition is same as in Example 1.
Embodiment 4
Only changing the molar fraction in formula into x=0.5, other condition is same as in Example 1.
The dielectric loss variation with temperature of embodiment 1-4 is shown in Fig. 1, it can be seen that embodiment 1 is worked as LiBa2Nb5O15Addition when being 0.2mol%, ceramics sample is lost less than 0.02 within the temperature range of 99～365 DEG C, real Execute example 3 and work as LiBa2Nb5O15Addition when being 0.4mol%, ceramics sample is lost within the temperature range of 70～402 DEG C and is less than 0.02, when addition is 0.5mol%, it is temperature during 0.4mol% that the loss temperature range less than 0.02 is slightly less than addition Scope.LiBa is described2Nb5O15Addition increase in the range of certain is so that the dielectric loss temperature range less than 0.02 Widen, be successfully obtained the dielectric material under high-temperature with ultra-low loss.Fig. 2 is to be not added with LiBa in pottery2Nb5O15Jie Electrical loss varies with temperature figure, and now ceramics sample is only lost less than 0.02 within the temperature range of 119～242 DEG C.By right Ratio is learnt, LiBa2Nb5O15Interpolation can be significantly expanded loss less than 0.02 temperature range, make pottery the highest broader Keep ultralow dielectric loss in temperature range, be with a wide range of applications.
Embodiment 5:
(1) BaTiO is prepared3、Na0.5Bi0.5TiO3、LiBa2Nb5O15Standby: to weigh BaCO according to mol ratio 1:13And TiO2 Form mixture A；Na is weighed according to mol ratio 1:1:42CO3、Bi2O3And TiO2Form mixture B；Claim according to mol ratio 4:1:5 Take BaCO3, Li2CO3And Nb2O5Form mixture C；
(2) taking mixture A, B, C, respectively with zirconium ballstone and deionized water, according to mass ratio 1:2:1, mixing and ball milling 3h is also 70 DEG C of drying, A in 1050 DEG C of calcinings, prepares powder body BaTiO in 820 DEG C of calcinings, C in 1120 DEG C of calcinings, B respectively3、 Na0.5Bi0.5TiO3、LiBa2Nb5O15；
(3) the powder body BaTiO that step (2) is obtained3、Na0.5Bi0.5TiO3And LiBa2Nb5O15According to 0.92Na0.5Bi0.5TiO3-0.08BaTiO3-xLiBa2Nb5O15Dispensing, wherein x=0.3, take mixture and deionized water, according to Mass ratio 1:2:1, mixing and ball milling 3h, 70 DEG C of drying, pelletizes, sieves, and forms granulation material；Wherein dry in material and add mass concentration Be 6% polyvinyl alcohol carry out pelletize, polyvinyl alcohol account for dry material quality 9.5%；
(4) step (3) gained granulation material is made under the pressure of 110MPa sample, first protect in the Muffle furnace of 650 DEG C Temperature 30min binder removal, then, is placed in the aluminium oxide saggar with zirconium oxide as backing plate in high temperature box furnace, heats up with 2 DEG C/min To 500 DEG C, it is warming up to 1150 DEG C with 5 DEG C/min and is incubated 2.5 hours, then, after being cooled to 500 DEG C with 5 DEG C/min, furnace cooling To room temperature；
(5), after the sample that polishing, cleaning step (4) sinter, silver electrode paste is uniformly coated at sample tow sides, in 650 DEG C sinter 40 minutes, obtain NBT base high-temperature low-loss ceramic capacitor.
Embodiment 6:
(1) BaTiO is prepared3、Na0.5Bi0.5TiO3、LiBa2Nb5O15Standby: to weigh BaCO according to mol ratio 1:13And TiO2 Form mixture A；Na is weighed according to mol ratio 1:1:42CO3、Bi2O3And TiO2Form mixture B；Claim according to mol ratio 4:1:5 Take BaCO3, Li2CO3And Nb2O5Form mixture C；
(2) mixture A, B, C are taken, respectively with zirconium ballstone and deionized water, according to mass ratio 1:1.5:1, mixing and ball milling 3.5h 80 DEG C of drying, A in 1100 DEG C of calcinings, prepares powder body BaTiO in 800 DEG C of calcinings, C in 1140 DEG C of calcinings, B respectively3、 Na0.5Bi0.5TiO3、LiBa2Nb5O15；
(3) the powder body BaTiO that step (2) is obtained3、Na0.5Bi0.5TiO3And LiBa2Nb5O15According to 0.92Na0.5Bi0.5TiO3-0.08BaTiO3-xLiBa2Nb5O15Dispensing, wherein x=0.4, take mixture and deionized water, according to Mass ratio 1:1.5:1, mixing and ball milling 3.5h, 80 DEG C of drying, pelletizes, sieves, and forms granulation material；Wherein dry in material and add quality Concentration be 5.5% polyvinyl alcohol carry out pelletize, polyvinyl alcohol account for dry material quality 10%；
(4) step (3) gained granulation material is made under the pressure of 110MPa sample, first protect in the Muffle furnace of 700 DEG C Temperature 35min binder removal, then, is placed in the aluminium oxide saggar with zirconium oxide as backing plate in high temperature box furnace, heats up with 2 DEG C/min To 500 DEG C, it is warming up to 1130 DEG C with 5 DEG C/min and is incubated 3 hours, then, after being cooled to 500 DEG C with 5 DEG C/min, cool to the furnace Room temperature；
(5), after the sample that polishing, cleaning step (4) sinter, silver electrode paste is uniformly coated at sample tow sides, in 620 DEG C sinter 35 minutes, obtain NBT base high-temperature low-loss ceramic capacitor.
Embodiment 7:
(1) BaTiO is prepared3、Na0.5Bi0.5TiO3、LiBa2Nb5O15Standby: to weigh BaCO according to mol ratio 1:13And TiO2 Form mixture A；Na is weighed according to mol ratio 1:1:42CO3、Bi2O3And TiO2Form mixture B；Claim according to mol ratio 4:1:5 Take BaCO3, Li2CO3And Nb2O5Form mixture C；
(2) taking mixture A, B, C, respectively with zirconium ballstone and deionized water, according to mass ratio 1:2:1, mixing and ball milling 3h is also 75 DEG C of drying, A in 1080 DEG C of calcinings, prepares powder body BaTiO in 840 DEG C of calcinings, C in 1130 DEG C of calcinings, B respectively3、 Na0.5Bi0.5TiO3、LiBa2Nb5O15；
(3) the powder body BaTiO that step (2) is obtained3、Na0.5Bi0.5TiO3And LiBa2Nb5O15According to 0.92Na0.5Bi0.5TiO3-0.08BaTiO3-xLiBa2Nb5O15Dispensing, wherein x=0.5, take mixture and deionized water, according to Mass ratio 1:2:1 mixing and ball milling 3h, 75 DEG C of drying, pelletizes, sieve, form granulation material；Wherein dry in material and add mass concentration Be 5% polyvinyl alcohol carry out pelletize, polyvinyl alcohol account for dry material quality 10%；
(4) step (3) gained granulation material is made under the pressure of 120MPa sample, first protect in the Muffle furnace of 680 DEG C Temperature 32min binder removal, then, is placed in the aluminium oxide saggar with zirconium oxide as backing plate in high temperature box furnace, heats up with 2 DEG C/min To 500 DEG C, it is warming up to 1140 DEG C with 5 DEG C/min and is incubated 2 hours, then, after being cooled to 500 DEG C with 5 DEG C/min, cool to the furnace Room temperature；
(5), after the sample that polishing, cleaning step (4) sinter, silver electrode paste is uniformly coated at sample tow sides, in 640 DEG C sinter 32 minutes, obtain NBT base high-temperature low-loss ceramic capacitor.
Above are only several detailed description of the invention of the present invention, the raw material of the present invention and the bound value of technological parameter are all The present invention can be realized, be illustrated the most one by one at this.

Claims (10)

1. a preparation method for NBT base high-temperature low-loss ceramic capacitor, has following steps:
(1) it is 0.92Na according to stoichiometric proportion0.5Bi0.5TiO3-0.08BaTiO3-xLiBa2Nb5O15, take BaTiO3Powder body, Na0.5Bi0.5TiO3Powder body and LiBa2Nb5O15Powder body mixes, and the mixture obtained is carried out ball milling, drying, pelletize and mistake After sieve, forming screening material, wherein x represents molar fraction, 0.2≤x≤0.5；
(2) step (1) gained screening material is made sample, sample is sintered 1120～1150 DEG C of insulations for 2～3 hours, It is then cooled to room temperature；
(3), after the sample that polishing cleaning step (2) sinter, silver electrode paste is uniformly coated at sample tow sides, in 600 ～650 DEG C sinter 30～40 minutes, obtain NBT base high-temperature low-loss ceramic capacitor.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 1, it is characterised in that: BaTiO3The preparation process of powder body includes: is first according to mol ratio 1:1 and weighs BaCO3And TiO2Form mixture A, take mixture A It is 1:(1～2 with zirconium ballstone and deionized water according to mass ratio): 1 mixing and ball milling 3～4h, and 60～80 DEG C of drying, then at 1120～1150 DEG C of calcinings, prepare BaTiO3Powder body.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 1, it is characterised in that: Na0.5Bi0.5TiO3The preparation process of powder body includes: is first according to mol ratio 1:1:4 and weighs Na2CO3、Bi2O3And TiO2Formed mixed Compound B, takes mixture B and zirconium ballstone and deionized water is 1:(1～2 according to mass ratio): 1 mixing and ball milling 3～4h, and 60～ 80 DEG C of drying, then at 800～850 DEG C of calcinings, prepare Na0.5Bi0.5TiO3Powder body.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 1, it is characterised in that: LiBa2Nb5O15The preparation process of powder body includes: is first according to mol ratio 4:1:5 and weighs BaCO3, Li2CO3And Nb2O5Form mixing Thing C, takes mixture C and zirconium ballstone and deionized water is 1:(1～2 according to mass ratio): 1 mixing and ball milling 3～4h 60～80 DEG C dry, then at 1000～1100 DEG C of calcinings, prepared LiBa2Nb5O15Powder body.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 1, it is characterised in that: x =0.2,0.3,0.4 or 0.5.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 1, it is characterised in that: Drying temperature in step (1) is 60～80 DEG C.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 1, it is characterised in that: In step (1), after mixture, zirconium ballstone and deionized water mixing, ball milling, drying formed dry material, by mass concentration be 5～ The binding agent of 6% adds and carries out pelletize to drying material, obtains granulation material, and binding agent accounts for dries the 9～10% of material quality.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 7, it is characterised in that: Sieving in step (1) is granulation material to be crossed 40 mesh and 80 mesh sieves respectively take middle material, it is thus achieved that screening material；Screening in step (2) Material makes sample under the pressure of 110～120MPa.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 1, it is characterised in that: In step (2), sample first carry out binder removal process be sintered again, binder removal process be by sample in the Muffle furnace of 600～700 DEG C Insulation 30～40min.
The preparation method of a kind of NBT base high-temperature low-loss ceramic capacitor the most as claimed in claim 1, it is characterised in that: In step (2), sample is placed in the aluminium oxide saggar with zirconium oxide as backing plate in high temperature box furnace, is warming up to 2 DEG C/min 500 DEG C, then it is warming up to 1120～1150 DEG C of insulations 2～3 hours with 5 DEG C/min, after being finally cooled to 500 DEG C with 5 DEG C/min, with Stove is cooled to room temperature.
CN201610370589.3A 2016-05-30 2016-05-30 Preparation method of NBT-based high-temperature low-loss ceramic capacitor Pending CN106045500A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610370589.3A CN106045500A (en) 2016-05-30 2016-05-30 Preparation method of NBT-based high-temperature low-loss ceramic capacitor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610370589.3A CN106045500A (en) 2016-05-30 2016-05-30 Preparation method of NBT-based high-temperature low-loss ceramic capacitor

Publications (1)

Publication Number Publication Date
CN106045500A true CN106045500A (en) 2016-10-26

Family

ID=57172146

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610370589.3A Pending CN106045500A (en) 2016-05-30 2016-05-30 Preparation method of NBT-based high-temperature low-loss ceramic capacitor

Country Status (1)

Country Link
CN (1) CN106045500A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107721412A (en) * 2017-11-13 2018-02-23 陕西科技大学 A kind of NBT based semiconductor ceramics and preparation method thereof
CN112159223A (en) * 2020-09-25 2021-01-01 陕西科技大学 High-temperature-stability high-dielectric-constant low-loss dielectric ceramic material, and preparation method and application thereof
CN113321506A (en) * 2021-07-08 2021-08-31 陕西科技大学 Lead-free relaxor ferroelectric ceramic material and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85100513A (en) * 1985-04-01 1986-08-13 中国科学院上海硅酸盐研究所 Bi-Na-Ba-TiO 3 series piezoelectric ceramic material for ultrasonic devices
CN1562876A (en) * 2004-03-30 2005-01-12 中国科学院上海硅酸盐研究所 Piezoelectric ceramics of modified barium natrium bismuth titanate doped in use for miniwatt ultrasonic transducer and preparation method
CN102173788A (en) * 2011-01-27 2011-09-07 西北工业大学 Sodium bismuth titanate-based high-strain lead-free piezoelectric ceramic and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85100513A (en) * 1985-04-01 1986-08-13 中国科学院上海硅酸盐研究所 Bi-Na-Ba-TiO 3 series piezoelectric ceramic material for ultrasonic devices
CN1562876A (en) * 2004-03-30 2005-01-12 中国科学院上海硅酸盐研究所 Piezoelectric ceramics of modified barium natrium bismuth titanate doped in use for miniwatt ultrasonic transducer and preparation method
CN102173788A (en) * 2011-01-27 2011-09-07 西北工业大学 Sodium bismuth titanate-based high-strain lead-free piezoelectric ceramic and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YURONG WU ET AL.: "The relaxor behavior and dielectric temperature stability of 0.85BaTiO3–0.15Na0.5Bi0.5TiO3–xLiBa2Nb5O15 ceramics", 《MATERIALS LETTERS》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107721412A (en) * 2017-11-13 2018-02-23 陕西科技大学 A kind of NBT based semiconductor ceramics and preparation method thereof
CN112159223A (en) * 2020-09-25 2021-01-01 陕西科技大学 High-temperature-stability high-dielectric-constant low-loss dielectric ceramic material, and preparation method and application thereof
CN113321506A (en) * 2021-07-08 2021-08-31 陕西科技大学 Lead-free relaxor ferroelectric ceramic material and preparation method thereof

Similar Documents

Publication Publication Date Title
CN103342556A (en) Preparation method of two-phase low-temperature co-sintered temperature stable dielectric ceramic material
CN102674832B (en) Barium-titanate-base lead-free bismuth-containing relaxation ferroelectric ceramic material and preparation method thereof
CN101811866B (en) Novel lead-free X8R type capacitor ceramic material and preparation method thereof
CN103011805B (en) BaTiO3 based leadless X8R type ceramic capacitor dielectric material and preparation method thereof
CN106045500A (en) Preparation method of NBT-based high-temperature low-loss ceramic capacitor
CN102992756B (en) X8R-type capacitor ceramic material with high dielectric constant and preparation method thereof
CN111995383A (en) Mg2-xMxSiO4-CaTiO3Composite microwave dielectric ceramic and preparation method thereof
CN111004030B (en) MgTiO (magnesium-titanium-oxide) powder3Microwave-based dielectric ceramic and preparation method thereof
CN102976748B (en) High-density barium strontium titanate ceramic and preparation method thereof
CN105174944A (en) Ultra-wide-temperature high-stability lead-free capacitor ceramic dielectric material and preparation method thereof
CN104058741A (en) Medium ceramic with stable ultra-wide temperature and preparation method thereof
CN111925187A (en) Lead-free high-pressure medium-temperature sintered strontium bismuth titanium-based dielectric material and preparation method thereof
CN104030678B (en) A kind of BaTiO 3base unleaded relaxation type ceramic dielectric material and preparation method thereof
CN104291811A (en) Preparation method of ceramic capacitor dielectric with high dielectric constant and superwide working temperature
CN102976750A (en) MgO-modified lead zirconate titanate pyroelectric ceramic material and preparation method thereof
CN103864416A (en) Method for preparing barium titanate ceramic capacitor medium at low sintering temperature
CN102515746A (en) Microwave dielectrically-adjustable material of barium strontium titanate composite molybdate and preparation method for same
CN104725036B (en) A kind of barium-strontium titanate-based energy storage ceramic of high temperature low loss and preparation method thereof
CN105367052B (en) A kind of high-temperature ceramic capacitor dielectric material and preparation method thereof
CN102531579B (en) Ceramic dielectric material and manufacture method thereof and ceramic capacitor and manufacture method thereof
CN101723665B (en) High-temperature stability dielectric ceramics capable of being sintered at intermediate temperature and preparation method thereof
CN104291821A (en) Preparation method of potassium-sodium niobate-based multilayer ceramic capacitor dielectric material
CN110304916A (en) A kind of anti-reduction BaTiO3Base media ceramic and preparation method
CN104310999A (en) Preparation method of low-temperature sintered X8R type ceramic capacitor medium
CN109650886A (en) A kind of Ba-Mg-Ta system LTCC material and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20161026

WD01 Invention patent application deemed withdrawn after publication