CN105906341A - Preparation method of single-phase structured nanometer sodium bismuth titanate ceramic powder - Google Patents

Preparation method of single-phase structured nanometer sodium bismuth titanate ceramic powder Download PDF

Info

Publication number
CN105906341A
CN105906341A CN201610225735.3A CN201610225735A CN105906341A CN 105906341 A CN105906341 A CN 105906341A CN 201610225735 A CN201610225735 A CN 201610225735A CN 105906341 A CN105906341 A CN 105906341A
Authority
CN
China
Prior art keywords
powder
ceramic powder
preparation
titanate ceramic
phase structure
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
CN201610225735.3A
Other languages
Chinese (zh)
Inventor
王静
荣桂娟
程海燕
李娜
江琦
王萌萌
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.)
Hebei University
Original Assignee
Hebei University
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 Hebei University filed Critical Hebei University
Priority to CN201610225735.3A priority Critical patent/CN105906341A/en
Publication of CN105906341A publication Critical patent/CN105906341A/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
    • C04B35/622—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
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/76—Crystal structural characteristics, e.g. symmetry
    • 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
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/781—Nanograined materials, i.e. having grain sizes below 100 nm
    • 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
    • C04B2235/74—Physical characteristics
    • C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
    • C04B2235/785—Submicron sized grains, i.e. from 0,1 to 1 micron

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a preparation method of single-phase structured nanometer sodium bismuth titanate ceramic powder. The preparation method comprises the following steps: 1, slowly adding TiCl4 to distilled water in proportion in a dropwise manner, slowly adding concentrated ammonia water to adjust the pH value to 6-8 and generate a precipitate, carrying out vacuum pumping filtration, and washing the obtained precipitate to obtain a TiO2 filter cake; 2, putting NaOH, Bi2O3 and the TiO2 filter cake in a mortar, grinding above materials for 1-3h to fully react the raw materials, adjusting the pH value to 6-8 by using an aqueous acetic acid solution, and drying the obtained reaction product to obtain powder; and 3, keeping the temperature of the powder obtained in step 2 unchanged in a range of 500-800DEG C for 0.5-3h to obtain the single-phase structured nanometer sodium bismuth titanate ceramic powder. The preparation method has the advantages of simplicity, simple operation, short reaction time, low cost, and suitableness for large-batch production. The nanometer sodium bismuth titanate leadless piezoelectric ceramic powder prepared through adopting the method mainly has the following advantages: 1, the ceramic powder is a single-phase structured pure ceramic powder; and 2, the particle sizes of the powder is uniform, the granularity of the powder is small, and the dimension of powder particles is about 200nm.

Description

The preparation method of the nanoscale bismuth-sodium titanate ceramic powder of phase structure
Technical field
The present invention relates to the preparation technology of leadless piezoelectric ceramics porcelain powder, the preparation method of the nanoscale bismuth-sodium titanate ceramic powder of a kind of phase structure.
Background technology
The crystalline material of voltage can occur when piezoelectric is affected by pressure effect between both ends of the surface.Piezoelectric mainly divides inorganic piezoelectric material and organic piezoelectric materials, and wherein, inorganic piezoelectric material is divided into again piezoquartz and piezoelectric ceramics, and piezoquartz refers generally to piezoelectric single crystal, and piezoelectric ceramics then refers to piezoelectricity polycrystal.Traditional piezoelectric ceramics is mainly based on leaded lead zirconate titanate (PZT) based material, and its main component is lead oxide (more than 60 ~ 70%).Lead oxide is a kind of volatile noxious substance, in the processing procedure after producing, using and be discarded, causes damage all can to the mankind and ecological environment.The volatilization of PbO will also result in the deviation of the stoichiometric proportion in pottery, makes the concordance of product and repeatability reduce, needs sealed sintering, make cost improve.
Development green material and technology are one of research tendencies of material science, piezoceramic material is applied the most universal in daily life, therefore, research and develop high performance leadless piezoelectric ceramics and there is very important scientific meaning and the urgent market demand, be increasingly becoming the focus of research.
Under existing conditions, research worker is seeking a kind of leadless piezoelectric material material that can replace Pb based system.In the middle of numerous piezoelectrics, bismuth-sodium titanate ((Na1/2Bi1/2)TiO3, NBT) show one's talent, the piezoelectric property that it is good, cause the interest of researcher.
NBT is that Smolenskii in 1961 et al. synthesizes first and finds.Along with the development leadless piezoelectric ceramics NBT sill of science and technology plays an important role in application.Due to big displacement, heavily stressed, low energy consumption, low cost, it is widely used to the fields such as accelerometer, supersonic motor, resonator, microfluidic separation device, ultrasonic transducer.NBT is important lead-free ferroelectric material, has ABO3Perovskite type ferroelectric character, it has big residual polarization, high Curie temperature Tc=320 DEG C, and has more complicated phase transformation sequence, 540oAbout C, NBT are Emission in Cubic (C, Pm3m)；320oTetragonal (T, P4bm), under room temperature, Bi it is changed into during C3+And Na+The R3c rhombic symmetry of complexity is had in A position.And NBT has good characteristics such as ferroelectricity is strong, piezoelectric modulus is big, dielectric constant is little, acoustical behavior is good, and its sintering temperature is relatively low it is considered to be the lead-free piezoceramic material body of most captivation.
The pattern of NBT ceramic powder, the uniformity etc. of chemical composition, directly affect composition and structure or even its electric property of ceramic material.The traditional preparation methods of NBT is solid sintering technology, and the shortcoming of this method is that granule is the most agglomerated together causes granular size heterogeneity.Other expert seminars are it is also proposed that other preparation methoies following, e.g., and molten-salt growth method, combustion method, hydro-thermal method, sol-gel process, chemical precipitation method etc..Molten-salt growth method preparation temperature is higher, and equipment requirements is the highest.Using organic solvent in combustion method, toxicity is relatively big more, and the cost of hydro-thermal method and sol-gel process is the highest and operation is complicated, and three of the above is unfavorable for industrialized production.And chemical precipitation method operation complexity, morphology control is general.
Summary of the invention
It is an object of the invention to provide the preparation method of the nanoscale bismuth-sodium titanate ceramic powder of a kind of phase structure, poor, the inhomogenous problem of granular size with the product pattern that the existing preparation method of solution exists, or the problem that existing method is unfavorable for industrialized production because cost is high, environment friendly is poor.
The object of the present invention is achieved like this:
A kind of preparation method of the nanoscale bismuth-sodium titanate ceramic powder of phase structure, it comprises the following steps:
1., by volume 10 ~ 12: 100, by TiCl4It is slowly dropped in distilled water, is then slowly added into the strong aqua ammonia of concentration 22 ~ 25%, adjust pH value to 6 ~ 8, produce precipitation, then vacuum filtration wash described precipitation, obtain TiO2Filter cake, standby；
2., by NaOH, Bi2O3With described TiO2Filter cake is put in mortar in the lump, grinds 1 ~ 3h, makes raw material fully react, and then adjusts pH value to 6 ~ 8 with the aqueous acetic acid of concentration 40 ~ 60%, dries, obtain powder body；
Wherein, with Bi2O3Na element meter contained by contained Bi element, NaOH, Na element and Bi element molar ratio are 0.5: 0.5 ＜ Na: Bi≤0.6: 0.4；With TiCl4Contained Ti element meter, Ti element is 1: 1 ＜ Ti: Na+Bi≤1: 1.2 with the molar ratio of described Bi element and the described total inventory of Na element；
3., step 2. gained powder body is incubated 0.5 ~ 3h under the conditions of 500 ~ 800 DEG C, obtains the nanoscale bismuth-sodium titanate ceramic powder of phase structure.
In the nanometer NBT raw powder's production technology of described phase structure, step 1. described in the time for adding of strong aqua ammonia control at 10 ~ 20min.
Preferably, in the nanometer NBT raw powder's production technology of described phase structure, step 1. described in the time for adding of strong aqua ammonia control at 14 ~ 16min, be preferably controlled at 15min.
Preferably, in the nanometer NBT raw powder's production technology of described phase structure, Na element and Bi element molar ratio are 0.55: 0.45≤Na: Bi≤0.6: 0.4；Ti element is 1: 1.05≤Ti: Na+Bi≤1: 1.2 with the molar ratio of described Bi element and the described total inventory of Na element.
It is furthermore preferred that Na element and Bi element molar ratio are Na: Bi=0.55: 0.45, Ti element is Ti: Na+Bi=1: 1.15 with the molar ratio of described Bi element and the described total inventory of Na element.
The preparation method of the present invention is easy, simple to operate, and the response time is relatively short, and expense cost is low, it is adaptable to large batch of production.The lead-free piezoelectric ceramic powder prepared relative to conventional solid sintering process, the method using the present invention prepares nanometer (submicron) bismuth-sodium titanate lead-free piezoelectric ceramic powder, mainly have the advantage that 1, true procelain powder for phase structure, 2, diameter of particle uniform, granularity is little.
Accompanying drawing explanation
Figure 1Preparation method technological process of the present inventionFigure。
Figure 2The SEM photograph of the NBT powder body prepared by embodiment 1.
Figure 3The XRD spectrum of the NBT powder body prepared by embodiment 1Figure。
Figure 4The XRD spectrum of the NBT powder body prepared by comparative example 1Figure。
Figure 5The XRD spectrum of the NBT powder body prepared by embodiment 2Figure。
Figure 6The XRD spectrum of the NBT powder body prepared by comparative example 2Figure。
Figure 7The particle diameter distribution of the NBT powder body prepared by embodiment 1Figure。
Figure 8The particle diameter distribution of the NBT powder body prepared by comparative example 3Figure。
Figure 9The SEM scanning of the NBT powder body prepared by embodiment 1, embodiment 2, comparative example 1, comparative example 2Figure。
Detailed description of the invention
The present invention obtainsCountryNsfc Projects (51302061), Hebei Province Natural Science fund (2014201076),CountryLevel Students' Innovation training plan project (201510075011) and University Of Hebei postgraduate innovate the support of Funded Projects (X2016084).
Following example and comparative example agents useful for same be: TiCl4: analytical pure, city is available；Strong aqua ammonia: concentration 25%, city is available；Aqueous acetic acid: concentration of volume percent 50%, city is available；Bi2O3: analytical pure, city is available；NaOH: analytical pure, city is available.
Embodiment 1
First by 11mL TiCl4It is slowly dropped in 100mL distilled water, in this solution, is then slowly added dropwise strong aqua ammonia, adjust pH value to 7, make TiO2+Precipitation, then vacuum filtration, washing, obtain TiO2Filter cake；
By gained TiO2Filter cake and 12.057g Bi2O3With 2.530g NaOH mixed grinding 1 hour, make raw material fully react, then adjust pH value to 7 with aqueous acetic acid, then dry, obtain powder body；
Gained powder body is incubated 1 hour under the conditions of 800 DEG C, obtains nanometer NBT powder body.
In the present embodiment, strong aqua ammonia time for adding controls between 14 ~ 16min.
Nanometer bismuth titanate sodium powder body prepared by the present embodiment is carried out SEM electron-microscope scanning, resultSuch as figure 2Shown in, byFigure 2It can be seen that the NBT powder granule uniform particle sizes prepared by the present embodiment, particle diameter is at about 200nm.
Nanometer bismuth titanate sodium powder body prepared by the present embodiment is carried out XRD detection, resultSuch as figure 3Shown in, byFigure 3It can be seen that the NBT powder body that NBT powder body is phase structure prepared by the present embodiment, without other impurity.
Embodiment 2
First by 11mL TiCl4Being slowly dropped in 100mL distilled water, be then slowly added dropwise strong aqua ammonia in this solution, adjusting pH value is 7, makes TiO2+Precipitation, then vacuum filtration, washing, obtain TiO2Filter cake；
By gained TiO2Filter cake and 12.057g Bi2O3With 2.530g NaOH mixed grinding 1.0h, make raw material fully react, then adjust pH value to 7 with aqueous acetic acid, then dry, powder body；
Gained powder body is incubated 3 hours under the conditions of 800 DEG C, obtains nanometer NBT powder body.
In the present embodiment, strong aqua ammonia time for adding controls between 14 ~ 16min.
Nm acid bismuth sodium powder body prepared by the present embodiment is carried out XRD detection, resultSuch as figure 5Shown in, byFigure 5It can be seen that the NBT powder body that NBT powder body is phase structure prepared by the present embodiment, without other impurity.But SEMFigureDisplay, owing to temperature retention time is longer, powder granule diameter increased.
Embodiment 3
Compared with Example 1, in the present embodiment, Na element and Bi element molar ratio are 0.6: 0.4, and Na element and Bi element total amount are 1.2: 1 with Ti element molar ratio, and other conditions keep consistent with embodiment 1.
Embodiment 4
Compared with Example 1, in the present embodiment, Na element and Bi element molar ratio are 0.525: 0.475, and Na element and Bi element total amount are 1.05: 1 with Ti element molar ratio, and other conditions keep consistent with embodiment 1.
Nanometer NBT powder body prepared by embodiment 3 ~ 4 is carried out XRD detection and SEM scans, result shows to be phase structure at the bismuth-sodium titanate powder body prepared by the practical range of the inventive method, and powder grain uniform particle sizes, the most consistent with the powder body prepared by embodiment 1.
Embodiment 5
Compared with Example 1, the holding temperature of the present embodiment controls at 500 DEG C, and temperature retention time controls at 3h, and other conditions keep consistent with embodiment 1.
Embodiment 6
Compared with Example 1, the holding temperature of the present embodiment controls at 650 DEG C, and temperature retention time controls at 2h, and other conditions keep consistent with embodiment 1.
Nanometer NBT powder body prepared by embodiment 5 ~ 6 is carried out XRD detection, and result shows that prepared bismuth-sodium titanate powder body is phase structure, and powder granule uniform particle sizes, the most consistent with the powder body prepared by embodiment 1.
Comparative example 1
First by 11mL TiCl4Being slowly dropped in 100mL distilled water, be then slowly added dropwise strong aqua ammonia in this solution, strong aqua ammonia time for adding controls to adjust pH value to be 7 at 15min, makes TiO2+Precipitation, then vacuum filtration, washing, obtain TiO2Filter cake；
By gained TiO2Filter cake and 12.057g Bi2O3With 2.530g NaOH mixed grinding 0.5h, make raw material fully react, then adjust pH value to 7 with aqueous acetic acid, then dry, powder body；
Gained powder body is incubated 1 hour under the conditions of 800 DEG C, obtains nanometer NBT powder body.
Nanometer bismuth titanate sodium powder body prepared by this comparative example is carried out XRD detection, resultSuch as figure 4Shown in, byFigure 4It can be seen that the non-phase structure of prepared powder body, miscellaneous peak occur, this is owing to milling time is shorter, and prepared powder body contains unreacted Bi completely2O3。
Comparative example 2
First by 11mL TiCl4Being slowly dropped in 100mL distilled water, be then slowly added dropwise strong aqua ammonia in this solution, adjusting pH value is 7, makes TiO2+Precipitation, then vacuum filtration, washing, obtain TiO2Filter cake；
By gained TiO2Filter cake and 11.649g Bi2O3With 2g NaOH mixed grinding 1.0h, make raw material fully react, then adjust pH value to 7 with aqueous acetic acid, then dry, powder body；
Gained powder body is incubated 1 hour under the conditions of 800 DEG C, obtains nanometer NBT powder body.
In this comparative example, Bi element and Na element molar ratio are 1: 1, and Bi element and Na element sum are 1: 1 with Ti element molar ratio.
Nm acid bismuth sodium powder body prepared by this comparative example is carried out XRD detection, resultSuch as figure 6Shown in, byFigure 6It can be seen that the non-phase structure of NBT powder body prepared by this comparative example, miscellaneous peak occur, this is due to Bi in process of lapping2O3, NaOH have a small amount of volatilization so that the ratio of Ti increases relatively, so at XRDFigure InDisplay is containing Ti compound impurities.
ByFigure 9It can be seen that embodiment 1 ~ 2 and the bismuth-sodium titanate powder body prepared by comparative example 1 ~ 2 are in addition to size is slightly different, the uniformity of powder granule all ratios are more uniform, and uniformity is good.
Comparative example 3
First by 11mL TiCl4It is slowly dropped in 100mL distilled water, in this solution, is then slowly added dropwise strong aqua ammonia, adjust pH value to 7, make TiO2+Precipitation, then vacuum filtration, washing, obtain TiO2Filter cake；
By gained TiO2Filter cake and 12.057g Bi2O3With 2.530g NaOH mixed grinding 1 hour, make raw material fully react, then adjust pH value to 7 with aqueous acetic acid, then dry, obtain powder body；
Gained powder body is incubated 1 hour under the conditions of 800 DEG C, obtains nanometer NBT powder body.
In this comparative example, strong aqua ammonia time for adding controls between 4 ~ 6min.
Particle diameter distribution to the powder body prepared by embodiment 1 and this comparative example detects, and result is respectivelySuch as figure 7WithFigure 8AndTable 1WithTable 2Shown in.
Table 1: the bismuth-sodium titanate diameter of particle statistics prepared by embodiment 1Table
Table 2: the bismuth-sodium titanate diameter of particle statistical table prepared by comparative example 3
ByFigure 7WithFigure 8To whenTable 1WithTable 2Contrast is it can be seen that more uniform according to the powder granule particle diameter prepared by the method for the present invention, and the powder granule size prepared by comparative example 3 differs, and particle size distribution range is wider.
Bismuth-sodium titanate powder granule prepared by this comparative example carries out SEM scanning and XRD detection, and result shows, the bismuth-sodium titanate powder body prepared by this comparative example is phase structure.

Claims (4)

1. a preparation method for the nanoscale bismuth-sodium titanate ceramic powder of phase structure, is characterized in that, comprise the following steps:
1., by volume 10 ~ 12: 100, by TiCl4It is slowly dropped in distilled water, is then slowly added into the strong aqua ammonia of concentration 22 ~ 25%, adjust pH value to 6 ~ 8, produce precipitation, then vacuum filtration wash described precipitation, obtain TiO2Filter cake, standby；
2., by NaOH, Bi2O3With described TiO2Filter cake is put in mortar in the lump, grinds 1 ~ 3h, makes raw material fully react, and then adjusts pH value to 6 ~ 8 with the aqueous acetic acid of concentration 40 ~ 60%, dries, obtain powder body；
Wherein, with Bi2O3Na element meter contained by contained Bi element, NaOH, Na element and Bi element molar ratio are 0.5: 0.5 ＜ Na: Bi≤0.6: 0.4；With TiCl4Contained Ti element meter, Ti element is 1: 1 ＜ Ti: Na+Bi≤1: 1.2 with the molar ratio of described Bi element and the described total inventory of Na element；
3., step 2. gained powder body is incubated 0.5 ~ 3h under the conditions of 500 ~ 800 DEG C, obtains the nanoscale bismuth-sodium titanate ceramic powder of phase structure.
The preparation method of the nanoscale bismuth-sodium titanate ceramic powder of phase structure the most according to claim 1, is characterized in that, step 1. described in the time for adding of strong aqua ammonia control at 10 ~ 20min.
The preparation method of the nanoscale bismuth-sodium titanate ceramic powder of phase structure the most according to claim 2, is characterized in that, step 1. described in the time for adding of strong aqua ammonia control at 14 ~ 16min.
The preparation method of the nanoscale bismuth-sodium titanate ceramic powder of phase structure the most according to claim 1, is characterized in that, Na element and Bi element molar ratio are 0.55: 0.45≤Na: Bi≤0.6: 0.4；Ti element is 1: 1.05≤Ti: Na+Bi≤1: 1.2 with the molar ratio of described Bi element and the described total inventory of Na element.
CN201610225735.3A 2016-04-13 2016-04-13 Preparation method of single-phase structured nanometer sodium bismuth titanate ceramic powder Pending CN105906341A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610225735.3A CN105906341A (en) 2016-04-13 2016-04-13 Preparation method of single-phase structured nanometer sodium bismuth titanate ceramic powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610225735.3A CN105906341A (en) 2016-04-13 2016-04-13 Preparation method of single-phase structured nanometer sodium bismuth titanate ceramic powder

Publications (1)

Publication Number Publication Date
CN105906341A true CN105906341A (en) 2016-08-31

Family

ID=56746051

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610225735.3A Pending CN105906341A (en) 2016-04-13 2016-04-13 Preparation method of single-phase structured nanometer sodium bismuth titanate ceramic powder

Country Status (1)

Country Link
CN (1) CN105906341A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113113582A (en) * 2021-03-19 2021-07-13 上海利物盛纳米科技有限公司 Preparation method of graphene-titanate lead-acid battery electrode active substance additive with layered structure

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1562872A (en) * 2004-04-19 2005-01-12 北京工业大学 Method for preparing leadless piezoelectric ceramics Na0.5Bi0.5TiO3 nano line
CN101219893A (en) * 2008-01-24 2008-07-16 河北大学 Method for producing nano-barium titanate based PTCR porcelain powder with low-temperature solid-state reaction
CN102531582A (en) * 2011-12-29 2012-07-04 洛阳理工学院 Method for preparing sodium bismuth titanate nanometer sheet
CN105016723A (en) * 2015-07-01 2015-11-04 陕西科技大学 Method for preparation of pure phase Na1/2Bi1/2TiO3 ceramic powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1562872A (en) * 2004-04-19 2005-01-12 北京工业大学 Method for preparing leadless piezoelectric ceramics Na0.5Bi0.5TiO3 nano line
CN101219893A (en) * 2008-01-24 2008-07-16 河北大学 Method for producing nano-barium titanate based PTCR porcelain powder with low-temperature solid-state reaction
CN102531582A (en) * 2011-12-29 2012-07-04 洛阳理工学院 Method for preparing sodium bismuth titanate nanometer sheet
CN105016723A (en) * 2015-07-01 2015-11-04 陕西科技大学 Method for preparation of pure phase Na1/2Bi1/2TiO3 ceramic powder

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113113582A (en) * 2021-03-19 2021-07-13 上海利物盛纳米科技有限公司 Preparation method of graphene-titanate lead-acid battery electrode active substance additive with layered structure

Similar Documents

Publication Publication Date Title
EP2414303B1 (en) Ceramic, piezoelectric device, and production method thereof
CN105040090B (en) A kind of preparation method of core shell structure lead titanates strontium titanate monocrystal nano material
CN101618889B (en) Method for preparing lead titanate nano column automatically assembled by perovskite structure nano pieces
CN103102154B (en) Bi0.5Na0.5TiO3-BaTiO3-BiMg0.5Ti0.5O3 lead-free piezoelectric ceramic material
CN102925979B (en) Method for preparing perovskite lead titanate crystal nanosheet
CN101619494A (en) Method for preparing perovskite structure lead titanate monocrystal nano rod
CN103553605B (en) KNN-BF leadless piezoelectric ceramic and preparation method thereof
CN103541014A (en) Lead-free high-voltage active crystal material and preparation method thereof
CN106220169A (en) Modified lead nickle niobate lead titanate piezoelectric ceramics and preparation method thereof
CN110182855A (en) Rare earth doped PMN-PT relaxor ferroelectric raw powder's production technology
Chang et al. Formation mechanism of (001) oriented perovskite SrTiO3 microplatelets synthesized by topochemical microcrystal conversion
CN102923766B (en) Preparation method of lead-titanate ceramic single-crystal nanosheet
Qin et al. The piezoelectric properties of transparent 0.75 Pb (Mg1/3Nb2/3) O3-0.25 PbTiO3: Pr3+ ceramics
CN106810238B (en) rare earth doped bismuth titanate nanocrystalline films with different morphologies and preparation method thereof
JP6312752B2 (en) Pure-phase multi-component production method, ceramic material based on pure-phase multi-component system, and molded bodies and composites formed therefrom
CN101831710A (en) Method for preparing lead titanate monocrystal nanometer branch crystal with perovskite structure
CN105906341A (en) Preparation method of single-phase structured nanometer sodium bismuth titanate ceramic powder
CN101386426B (en) Method for preparing leadless piezoelectric potassium sodium niobate film
CN106892450B (en) One kind synthesizing PbTiO by La ion dopings3The method of disk
CN103086715A (en) Preparation method of lead zirconate-titanate piezoelectric ceramic powder
Omran et al. Influence of PbO phase content on structural and optical properties of PZT nanopowders
CN101077837B (en) Neodymium and vanadium composite doping bismuth titanate powder and preparation method thereof
CN105732024A (en) Novel binary K0.5Bi0.5TiO3-BiMg0.5Zr0.5O3 leadless piezoelectric ceramic material and preparation
CN101269974B (en) Synthesis method for preparing perovskite series ceramic nano-powder body with texture lamellar structure
CN107540373A (en) A kind of La ion dopings PZT based piezoelectric ceramic materials 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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160831