CN1765826A - The preparation method of Nd-doped bismuth titanate super fine powder - Google Patents

The preparation method of Nd-doped bismuth titanate super fine powder Download PDF

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CN1765826A
CN1765826A CN 200510029280 CN200510029280A CN1765826A CN 1765826 A CN1765826 A CN 1765826A CN 200510029280 CN200510029280 CN 200510029280 CN 200510029280 A CN200510029280 A CN 200510029280A CN 1765826 A CN1765826 A CN 1765826A
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bismuth titanate
preparation
fine powder
doped bismuth
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CN100358836C (en
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阚艳梅
王佩玲
张国军
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The present invention relates to a kind of preparation method of Nd-doped bismuth titanate super fine powder.Be characterised in that: partly replace bismuth in the bismuth titanates with neodymium, adopt hydrolysis method to prepare particle diameter little (100-200nm), the uniform Nd-doped bismuth titanate powder of particle size distribution, with the pressureless sintering in air of this powder, obtain densification, dielectric properties and the good bismuth titanate based function ceramics of piezoelectric property.The raw material that adopts is that purity is not less than chemical pure Neodymium trioxide (Nd 2O 3), five water Bismuth trinitrate (Bi (NO 3) 35H 2O), butyl (tetra) titanate (Ti (OC 4H 9) 4) and nitric acid (HNO 3), the mole number that finally obtains neodymium in powder and the pottery is in the 0.1-1.0 scope, and the relative density of pottery is higher than 97%, and dielectric loss is lower than 1.0% under the room temperature.

Description

The preparation method of Nd-doped bismuth titanate super fine powder
Technical field
That the present invention relates to is the preparation method of a kind of Nd-doped bismuth titanate (Nd-BIT) superfine powder.More precisely provide a kind of with Neodymium trioxide (Nd 2O 3), five water Bismuth trinitrate (Bi (NO 3) 35H 2O) and butyl (tetra) titanate (Ti (OC 4H 9) 4) be raw material, adopt hydrolysis method to prepare presoma, after the thermal synthesis reaction, obtain the adulterated bismuth titanate super fine powder of neodymium.Use this powder can obtain densification, Nd-doped bismuth titanate base pottery that electrical property is good, belong to the functional ceramic powder preparation field by pressureless sintering.
Background technology
Bismuth titanates (Bi 4Ti 3O 12) be to have perovskite structure to contain the ferroelectrics that structure in the bismuth layer-like compound extended familys is the simplest, study at most.It has low-k, high curie point and big characteristics such as spontaneous polarization, and at electrical condenser, aspects such as high-temperature piezoelectric transmitter and photoelectric device have wide practical use.In addition, from environment protection and Sustainable development angle, the advantage that bismuth titanate based pottery does not contain lead element makes it might become the potential surrogate of the Pb-based lanthanumdoped zirconate titanates base piezoelectric ceramic of present widespread use.Yet the sheet structure characteristics determined of bismuth titanates its tender stupid electric field height, be difficult for polarization.In addition, also there is the high and big shortcoming of loss of leakage conductance electric current in bismuth titanate ceramics.
Recently, because ferroelectric material may use in permanent random access memory (Non-volatile Ramdom AccessMemories), caused the very big interest of people to ferroelectric material, wherein the bismuth titanate based material of trivalent rare earth element replacement part bismuth has very big development potentiality.1999 and 2002 are at Nature[1, B.H.Park, B.S.Kang, S.D.Bu, T.W.Noh, J.Lee and W.Jo, Nature, 401 (1999) 682.] and Science[2, H.N.Lee, D.Hesse, N.Zakharov and U.G sele, Science, 296 (2002) 2006.] on the lanthanum of mixing bismuth titanates (Bi is arranged respectively 3.25La 0.75Ti 3O 12) the research report of film.Find that the bismuth titanate film after the lanthanum modification shows good saturated ferroelectric hysteresis loop and very strong stability, and have good anti-fatigue ability, under 1MHz, read and write 3 * 10 10Inferior not aging yet, show that it is a kind of potential high-quality ferroelectric random storage material.
In general, the performance of powder can have influence on the performance of final material usually, and powder synthetic method the most frequently used for bismuth titanate based pottery is a solid reaction process, soon mixes with the corresponding oxide compound of material component, and calcining is synthetic at a certain temperature then.Though this method is simple, powder synthesis temperature height, the densification degree that particle diameter is big, phase composite is difficult to simplification, sintering temperature height and material are low.With the bismuth titanates is example, and the sintering temperature that adopts the solid state reaction synthetic powder is usually above 1050 ℃, and the relative density of material is lower than 95%, and because the sintering temperature height causes Bi usually 2O 3Volatilization, in material, form a large amount of defectives and influence its performance.Therefore, adopt wet chemistry method to prepare the sintering activity that the little ceramic powder of particle diameter will help improving powder, obtain the high stupalith of densification degree.
Relevant Bi 4Ti 3O 12The research of pottery doping vario-property is of long duration, but forefathers are mainly by adding Nb 5+, Sb 5+, Ta 5+And W 6+Reduce conductivity of electrolyte materials Deng donor impurity replacement titanium ion, improve the polarization performance [3, Y.Noguchi, I.Miwa, Y.Goshima and M.Miyayama, Jpn.J.Appl.Phys., 39 (2000) L1259.] of material.Though high price is entrained in the performance of material is improved; but because the radius of high valence ion and institute are electrically charged and substitution ion differs greatly; usually can cause its solid solution in bismuth titanates limited, in material, form easily second performance that influences material mutually.And trivalent rare earth ions has electricity price identical with bismuth ion and close ionic radius, can form continuous solid solution.Studies show that La is at Bi 4Ti 3O 12In solid solution can suppress the generation of intermediate phase in the calcination process, reduce grain growing speed and the octahedral vibration of remarkably influenced Ti-O, make the intensity of the octahedra shuttle belt of Ti-O in the infrared spectra and position that in various degree variation take place.On the other hand, La is at Bi 4Ti 3O 12In solid solution the densification degree of material is significantly improved, and suppress Bi 2O 3Volatilization, make conductivity of electrolyte materials and dielectric loss obviously reduce [4, Y.M.Kan, X.H.Jin, G J.Zhang, P.L.Wang, Y.B.Chen and D.S.Yan, J.Mater.Chem., 14 (2004) 3566.].Because Bi 4-xLn xTi 3O 12(Ln is a trivalent rare earth element) is by (Bi 2O 2) 2+Stratiform and breast uhligite stratiform [(Bi 2-xLa x) Ti 3O 10]] 2-Form along c direction of principal axis stacking, lanthanon can promote TiO to the replacement of bearing Bi element in the calcium titanium ore bed 6Therefore octahedral distortion, can be predicted, and more helps the raising of ferroelectric properties in bearing the uhligite stratiform less than the rare earth element replacement part Bi of La with ionic radius.
Summary of the invention
The object of the present invention is to provide a kind of have particle diameter little, be evenly distributed, the preparation method of Nd-doped bismuth titanate (Nd-BIT) powder that sintering activity is high.
Basic design of the present invention is Nd 3+With Bi 3+Institute is electrically charged identical, therefore at Bi 4Ti 3O 12Middle Nd 3+Easily replace Bi 3+Enter Bi 4Ti 3O 12Lattice.Again because Nd and La belong to trivalent rare earth element together, and Nd has different electronic configurations with La, and ionic radius is also slightly variant, and they enter Bi 4Ti 3O 12Can form different ligand fields behind the lattice, the lattice distortion degree that causes is also different, also can produce different influences to physicals.Except that additive types and components selection, the preparation technology of powder and performance thereof also have great influence to the final performance of sintered ceramic.Therefore, we are selecting Nd 2O 3In the time of as additive, adopt hydrolysis method to prepare superfine powder, obtain fine and close Nd-doped bismuth titanate (Nd-BIT) base ceramic material by pressureless sintering.
The objective of the invention is to implement: be not less than chemical pure Neodymium trioxide (Nd with purity by following manner 2O 3), five water Bismuth trinitrate (Bi (NO 3) 35H 2O) and butyl (tetra) titanate (Ti (OC 4H 9) 4) be starting raw material, adopt hydrolysis method to prepare the superfine powder of Nd-doped bismuth titanate (Nd-BIT).Obtain fine and close Nd-doped bismuth titanate (Nd-BIT) pottery by pressureless sintering.Prove the excellent specific property of the superfine powder of preparation.
Specifically:
The chemical constitution formula of Nd-doped bismuth titanate powder is Bi 4-xNd xTi 3O 12, 0.1≤x in the formula≤1.0,
(1) according to mole number design component in the 0.1-1.0 scope of neodymium.
(2) raw material: comprise that purity is not less than chemical pure Neodymium trioxide (Nd 2O 3), five water Bismuth trinitrate (Bi (NO 3) 35H 2O), butyl (tetra) titanate (Ti (OC 4H 9) 4Composition proportioning according to above-mentioned (1) is selected an amount of corresponding compounds.
(3) powder is synthetic: with Nd 2O 3And Bi (NO 3) 35H 2O is dissolved in respectively in the nitric acid of pH≤3 and obtains settled solution, spirituous solution with butyl (tetra) titanate is mixed to clarification under magnetic agitation again, adding deionized water then is hydrolyzed, the pH value to 9 that drips weak ammonia adjusting suspension at last fully precipitates to guarantee the solution metal ion, obtains the adulterated bismuth titanates of neodymium (Nd-BIT) presoma again behind washing-suction filtration.With the Nd-doped bismuth titanate powder of presoma in 400-800 ℃ of 0.5-1.0 hour synthetic designed component of calcining in air.
(4) has the Nd-doped bismuth titanate powder of different neodymium content through dry-pressing, cold isostatic compaction (forming pressure is 100-300MPa), then in air in 900-1100 ℃ of pressureless sintering, soaking time is controlled in 1-2 hour scope, makes fine and close Nd-doped bismuth titanate pottery.
Advantage of the present invention is:
(1) synthesis technique of powder is simple, and cost is low, does not need complex apparatus, enlarges scale production easily.
(2) particle diameter of synthetic powder is between 100-200nm, and is evenly distributed, and has high sintering activity, helps the densification of pottery.
(3) by regulating sintering condition, pressureless sintering can obtain relative density and be higher than 97% fine and close Nd-doped bismuth titanate pottery, this material has good dielectric, ferroelectric and piezoelectric property, thereby proves the mix excellent specific property of ultra-fine bismuth titanate powder of neodymium provided by the invention.
Description of drawings
Fig. 1 powder preparing process flow sheet
Fig. 2 consists of Bi 3.5Nd 0.5Ti 3O 12Transmission electron microscope (TEM) photo of presoma (a) (b) powder after 600 ℃/0.5h calcining
Fig. 3 (a) and (b) be respectively to consist of Bi 4-xNd xTi 3O 12(x=0.2,0.5,0.75) composes through the XRD figure of 600 ℃/0.5h and 750 ℃/0.5h calcining back powder respectively that (Si is interior mark among the figure, and all the other are Bi 4-xNd xTi 3O 12The peak)
Fig. 4 (a) and (b) be respectively to consist of Bi 3.5Nd 0.5Ti 3O 12The specific inductivity of pottery and the graph of a relation of dielectric loss and temperature
Fig. 5 consists of Bi 3.25Nd 0.75Ti 3O 12Scanning electron microscope (SEM) photo (a) and ferroelectric hysteresis loop (b)
Embodiment
Embodiment 1 is with five water Bismuth trinitrate (Bi (NO 3) 35H 2O), Neodymium trioxide (Nd 2O 3) and butyl (tetra) titanate (Ti (OC 4H 9) 4) be initial feed, rare nitric acid and ethanol are solvent, preparation Nd-doped bismuth titanate presoma, its technical process is as shown in Figure 1.At first with Bi (NO 3) 35H 2O, Nd 2O 3Be dissolved in rare nitric acid and be mixed with settled solution, Bi (NO 3) 35H 2The dissolving of O in nitric acid belongs to endothermic process, can be by suitably heating promotion dissolving.Press Bi then 4-xNd xTi 3O 12The stoichiometric ratio of (x=0.2,0.5,0.75) is with Ti (OC 4H 9) 4Spirituous solution be added drop-wise in the solution for preparing above, be stirred to solution clarification.While stirring a large amount of deionized waters is poured into rapidly in this solution then, can be observed white precipitate and generate rapidly, drip proper ammonia at last again and regulate pH value to 9, to guarantee that reactant precipitates fully.The white precipitate of gained is through deionized water wash 4 times, in 90 ℃ of dryings, obtains the Nd-doped bismuth titanate presoma after the powder that grinds is crossed 100 mesh sieves after the washing with alcohol dehydration 1 time.Make Bi in 600 ℃ of calcinings in 8 hours 4-xNd xTi 3O 12, obtain the Nd-doped bismuth titanate pottery.The XRD figure spectrum of calcining powder respectively as shown in Figures 2 and 3 under the microstructure of the Nd-doped bismuth titanate powder of preparation and the differing temps
Neodymium content is 0.5 mole (x=O.5) in the final component of embodiment 2 design, prepares presoma according to the method for embodiment 1, through 600 ℃ of synthetic Bi of calcining 3.5Nd 0.5Ti 3O 12Powder, microstructure are as shown in Figure 2.
Embodiment 3 prepares presoma according to component and the method for embodiment 1, and the temperature lower calcination of 600 ℃ and 750 ℃ 0.5 hour, the XRD figure spectrum of gained powder as shown in Figure 3 respectively.
Neodymium content is 0.5 mole (x=0.5) in the final component of embodiment 4 design, prepares presoma according to the method for embodiment 1, through the synthetic Bi of 600 ℃/0.5h calcining 3.5Nd 0.5Ti 3O 12Powder, the preparation pottery, sintering temperature is 1000 ℃, soaking time is 2 hours.The Bi of preparation 3.5Nd 0.5Ti 3O 12The relation of ceramic dielectric constant and dielectric loss and temperature as shown in Figure 4.Bi among the figure 3.5Nd 0.5Ti 3O 12The specific inductivity of pottery and dielectric loss in the temperature range of room temperature-250 ℃ hardly the variation with temperature and frequency change, and loss is lower than 1.0%, and the specific inductivity of unadulterated bismuth titanates is subjected to the influence of temperature and frequency bigger, and the dielectric loss of room temperature is 2%-5% in the range of frequency of 10KHz～1MHz.
Neodymium content is 0.75 mole (x=0.75) in the final component of embodiment 5 design, prepares presoma according to the method for embodiment 1, through the synthetic Bi of 600 ℃/0.5h calcining 3.25Nd 0.75Ti 3O 12Powder, the preparation pottery, sintering temperature is 1000 ℃, soaking time is 2 hours.The Bi of preparation 3.25Nd 0.75Ti 3O 12Microstructure of ceramics and ferroelectric hysteresis loop are as shown in Figure 5.Know the remnant polarization (2P of the back material that mixes by ferroelectric hysteresis loop figure r) be 30 μ C/cm 2, and the 2P when not mixing rOnly be 16 μ C/cm 2

Claims (9)

1, a kind of preparation method of Nd-doped bismuth titanate super fine powder is characterized in that:
(1) with Nd 2O 3, Bi (NO 3) 35H 2O and Ti (OC 4H 9) 4Be raw material, by the Bi of design 4-xNd xTi 3O 12The chemical constitution weighing, 0.1≤x in the formula≤1.0;
(2) step (1) is weighed up the Nd of weight 2O 3And Bi (NO 3) 35H 2O is dissolved in respectively in the nitric acid of pH≤3 and obtains settled solution, again with the Ti (OC that weighs up weight 4H 9) 4Spirituous solution under magnetic agitation, be mixed to clarification;
(3) add deionized water and be hydrolyzed, obtain white depositions;
(4) last dropping ammonia is regulated the pH value to 9 of suspension, again through washing, dry, sieve after the adulterated bismuth titanates presoma of acquisition neodymium;
(5) presoma of step (4) gained is calcined the Nd-doped bismuth titanate powder of 0.5-1.0 hour thermal synthesis design component in 400-800 ℃ of air.
2, by the preparation method of the described Nd-doped bismuth titanate super fine powder of claim 1, it is characterized in that Nd as raw material 2O 3, Bi (NO 3) 35H 2O and Ti (OC 4H 9) 4Purity be not less than chemical pure.
3, by the preparation method of the described Nd-doped bismuth titanate super fine powder of claim 1, it is characterized in that the purity of described nitric acid or ammoniacal liquor is not less than chemical pure.
4, by the preparation method of the described Nd-doped bismuth titanate super fine powder of claim 1, it is characterized in that step (4) regulates pH to 9 back with the white precipitate of gained through ammoniacal liquor and use deionized water wash, washing with alcohol is dewatered then.
5, by the preparation method of the described Nd-doped bismuth titanate super fine powder of claim 4, it is characterized in that deionized water wash 4-6 time, use number of times 1-2 time of ethanol dehydration thereafter.
6, by the preparation method of the described Nd-doped bismuth titanate super fine powder of claim 1, it is characterized in that drying temperature is 85-95 ℃.
7,, it is characterized in that dry back powder becomes neodymium doping presoma behind 100 mesh sieves by the preparation method of the described Nd-doped bismuth titanate super fine powder of claim 1.
8, by the preparation method of the described Nd-doped bismuth titanate super fine powder of claim 1, it is characterized in that the Nd-doped bismuth titanate super fine powder particle diameter is between 100-200nm.
9, by the preparation method of the described Nd-doped bismuth titanate super fine powder of claim 1, it is characterized in that Bi 4-xNd xTi 3O 12X=0.2,0.5 or 0.75 in the chemical constitution formula.
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CN102267721A (en) * 2011-04-11 2011-12-07 山东建筑大学 Quick preparation method of perovskite-structure polycrystalline nanopowder with chemical formula of Ca0.4Sr0.6Bi4Ti4O15
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CN102517011A (en) * 2011-11-16 2012-06-27 陕西科技大学 Neodymium-doped bismuth titanate nanocrystalline upconversion material and preparation method thereof
CN102557619A (en) * 2011-12-28 2012-07-11 山东女子学院 Preparation method of high-orientation Ca0.4Sr0.6Bi4Ti4O15 template grain film
CN103159474A (en) * 2013-02-25 2013-06-19 中国科学院上海硅酸盐研究所 Antiferroelectric stored energy ceramic materials and ceramic element and preparation method
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US6107227A (en) * 1998-08-03 2000-08-22 Cts Corporation Barium neodymium titanate dielectric ceramic composition incorporating samarium oxide for improved electrical performance
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CN102267721A (en) * 2011-04-11 2011-12-07 山东建筑大学 Quick preparation method of perovskite-structure polycrystalline nanopowder with chemical formula of Ca0.4Sr0.6Bi4Ti4O15
CN102267812A (en) * 2011-04-11 2011-12-07 山东女子学院 Method for preparing thick membrane by using polycrystal Ca0.4Sr0.6Bi4Ti4O15 nano powder with perovskite structure
CN102267721B (en) * 2011-04-11 2013-06-19 山东建筑大学 Quick preparation method of perovskite-structure polycrystalline nanopowder with chemical formula of Ca0.4Sr0.6Bi4Ti4O15
CN102517011A (en) * 2011-11-16 2012-06-27 陕西科技大学 Neodymium-doped bismuth titanate nanocrystalline upconversion material and preparation method thereof
CN102557619A (en) * 2011-12-28 2012-07-11 山东女子学院 Preparation method of high-orientation Ca0.4Sr0.6Bi4Ti4O15 template grain film
CN102557619B (en) * 2011-12-28 2013-05-22 山东女子学院 Preparation method of high-orientation Ca0.4Sr0.6Bi4Ti4O15 template grain film
CN103159474A (en) * 2013-02-25 2013-06-19 中国科学院上海硅酸盐研究所 Antiferroelectric stored energy ceramic materials and ceramic element and preparation method
CN116371398A (en) * 2023-04-11 2023-07-04 中南大学 BIT-Nd block piezoelectric photocatalyst and preparation method and application thereof
CN116371398B (en) * 2023-04-11 2023-11-10 中南大学 BIT-Nd block piezoelectric photocatalyst and preparation method and application thereof

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