CN102093045A - Barium titanate and barium ferrite composite powder with nucleus shell structure and preparation method thereof - Google Patents
Barium titanate and barium ferrite composite powder with nucleus shell structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses barium titanate and barium ferrite composite powder with a nucleus shell structure and a preparation method thereof. The powder is ferroelectric-ferromagnetic multifunctional composite powder with a nucleus shell structure, wherein ferroelectric powder barium titanate serves as a nucleus; a controllable-thickness ferromagnetic shell layer made from barium ferrite is arranged outside the nucleus; and the thickness of a shell layer is adjustable between 10 nanometers and 100 nanometers. The preparation method of the powder is a uniform co-precipitation out-phase coating method. In a co-precipitation process, urea is taken as a precipitant, any surface modification on barium titanate is not required, the nucleus is coated fully by the shell layer, and independent shell layer particles do not exist in a product. The method has the advantages of low cost, easiness and convenience in operating, simple equipment, wide application range and suitability for mass production.
Description
Technical field
The present invention relates to a kind of ferroelectric-ferromagnetic multifunctional composite powder body material and preparation method thereof with nucleocapsid structure, more particularly say, a kind of nucleocapsid structure barium titanate-barium ferrite composite powder material and preparation method thereof belongs to Multifunction composite powder material field.
Background technology
The multifunctional composite powder body material is the hot fields of current research, and this class material integrates multiple physical chemistry functions such as magnetic, electrical, optical, heat, catalysis, has great importance for the microminiaturization of Device element, function intensification, environmental protection.
The multi-functional powder of ferroelectric-ferromagnetic is one to have the powder body material of ferroelectricity and ferromagnetic property roughly the same the time, wherein the product effect that is caused by the coupling between ferroelectric phase and the ferromagnetic phase makes it have huge application potential in microwave regime, high voltage electric transmission route survey, wide band detection, magnetic sensors and fields such as transmodulator, micro-nano device control, thereby has been subjected to the extensive concern of countries in the world.
Occurring in nature has ferroelectric and ferromagnetic property when existing monophase materials seldom is mainly bismuth perovskite-like, rare earth manganite and Fang Pengshi, and their magnetic electricity performance only exists under cold condition, and magneto-electric coupled coefficient is very low.Though the method that replaces by element doping and atom can improve the magneto-electric coupled coefficient and the working temperature of single-phase ferroelectric-ferromagnetic material, the large-scale practical application of its result's distance also has no small distance.
Therefore, adopt material compound thinking, sophisticated ferroelectrics and ferro-magnetic are carried out the compound important channel that just becomes preparation ferroelectric-ferromagnetic powder body material according to certain mode.For example people such as Yao Xi carries out physical mixed with ferroelectric powder and ferromagnetic powder, has obtained having simultaneously the composite powder material of ferroelectric-ferromagnetic performance.(Yao Xi.Ferroelectric and ferromagnetic microcrystalline glass ceramics.Ferroelectrics, 2001,261 (1): 3), Xie Shuhong adopts the method for collosol and gel electrostatic spinning to prepare the complex fiber material (CN101274844A) of ferroelectric-ferromagnetic.
In current ferroelectric-ferromagnetic matrix material, people often adopt the ferrite (AB of spinel structure
2O
4), and barium ferrite has higher saturation magnetization and magnetocrystalline anisotropic, thereby can overcome the snoek restriction easily plays a role in the high-frequency electromagnetic environment, at microwave absorbing material, perpendicular recording material and microwave and millimeter wave device material field have crucial status, if itself and ferroelectric phase are carried out compound, then be expected to further expand the range of application of ferroelectric-ferromagnetic material, produce more deep effect at magnetoelectricity cross complaint and field of energy conversion.
Mixing on the micro-nano-scale of realizing from simple physical mixed to sol-gel method, ferroelectric phase with ferromagnetic in the raising that matter has been arranged aspect the blended homogeneity.But only the method by physical mixed can't solve the composition segregation problem of this powder in the subsequent applications field; Simultaneously owing to a little less than the interaction between the two-phase, therefore can't make full use of the new physics-chem characteristic that coupling produced between the magnetoelectricity phase.For this reason, need the new complex method of exploitation badly.
Hud typed structure has advantages such as high stability, pattern, size, composition and controllable structure, can realize the fully effectively coupling of different components on micro-nano-scale, and can be by artificially therefore design and controlled preparation are considered to prepare the ideal structure form of ferroelectric-ferromagnetic multifunctional composite powder body material to satisfy many specific application requiring.V.Corral-Flores adopts the nucleocapsid structure form, make the magnetic-electric coefficient of the magnetic electric compound material (V.Corral-Flores that is significantly improved, Enhanced magnetoelectric effect in core-shell particulate composites, Journal of applied physics, 99,2006); C.A.F.Vaz etc. adopt the Fe of nucleocapsid structure
3O
4/ BaTiO
3(C.A.F.Vaz, J.Hoffman, A.-B.Posadas, C.H.Ahn, Magnetic anisotropy modulation of magnetite in Fe
3O
4/ BaTiO3 (100) epitaxial structures, Applied physics letters, 94,2009) realized the adjustable of magneticanisotropy.People such as ChaoWang are at BaFe
12O
19The surface of powder has coated one deck BaTiO
3, by nuclear (BaFe
12O
19) shell (BaTiO
3) between interaction realized the (ChaoWang that controls to the powder dielectric characteristics, Xijiang Han, Ping Xu, XiaohongWang, Xueai Li, Hongtao Zhao, Magnetic and dielectric properties of barium titanate-coated barium ferrite, Journal of Alloys and Compounds, 476,2009).
At present, the preparation method of hud typed structure powder mainly comprises sol-gel method (Chinese patent 200410041128.9, Chinese patent 200710171827.9, Chinese patent 200710100330.8, Chinese patent 200710040489.5), emulsion polymerization (Chinese patent 200510087784.7, Chinese patent 01105317.8, Chinese patent 200610125136.0), chemical reduction method (Chinese patent 200510028257.9, Chinese patent 200510049662.9), solvent-thermal method (Chinese patent 200710164855.8), self-assembly method (Chinese patent 200810123880.6, Chinese patent 200410018588.X) layer by layer, magnetron sputtering method (Chinese patent 200610015536.6) etc.
Yet all there is different shortcomings in aforesaid method self.For example: there is the high shortcoming of cost in sol-gel method because its metal alkoxide costs an arm and a leg; Emulsion polymerization, chemical reduction method and layer by layer self-assembly method relate to modification to nuclear core material surface so preparation process more complicated; And solvent-thermal method and magnetron sputtering rule having relatively high expectations to equipment.
The precipitator method have with low cost, advantage simple to operate.Prepare the powdered ceramics powder body material with the precipitator method and realized suitability for industrialized production.In recent years, adopt the precipitator method to prepare the attention that core-shell particles has caused people, Tang Fang adopts sedimentation at SiO thoroughly
2The surface has coated semi-conductor ZnO, TiO
2, prepared nucleocapsid structure composite powder material (CN1296917A) with specific physical; Chen Heguo etc. adopt the precipitator method at SiO
2The surface has coated stannic oxide (CN101613078A); People such as Yang Dean adopt coprecipitation method to prepare hud typed strontium/calcium hydroxyapatite nano powder (CN101428777); The polystyrene microsphere surface in situ growth hydrotalcite (CN101274769A) of chemical precipitation method after sulfonation such as Xu Sailong; Old build fixed wait with the precipitator method in the surface preparation of polystyrene microsphere Mn ferrite (CN101086911); The positive equality of Liu with co-electrodeposition method at the polystyrene Fe that has been the ball surface preparation
3O
4, obtained the magnetic microsphere (CN1718619A) of nucleocapsid structure.
Current employing chemical precipitation method prepares in numerous examples of core-shell particles, highly basic precipitation agent for example NaOH and the KOH of adopting more, make the degree of supersaturation of solution be difficult to control, precipitation coating process is followed a large amount of homogeneous phase nucleation processes, cause often being mixed with in the nucleocapsid powder a large amount of independent shell particles, product purity is restricted, and has also increased isolating difficulty.Though by to can being improved degree of purity of production by the surface treatment of coating particles, the organic coupling agent that surface treatment used cost an arm and a leg mostly, make cost increase; In addition, the extra surface treatment process that increases makes also that undoubtedly operation is more loaded down with trivial details.
Therefore, work out with low costly, simple to operate, be suitable for the coprecipitation method preparation technology of large-scale production, have great importance for the basic theory and the applied research of ferroelectric-ferromagnetic core-shell particles.
Summary of the invention
The purpose of this invention is to provide a kind of barium titanate-barium ferrite composite granule and even co-precipitation out-phase coating preparation method thereof.This material is the ferroelectric-ferromagnetic multifunctional composite powder body material with nucleocapsid structure, and its nuclear is ferroelectric powder material barium titanate, be the ferromegnetism shell with the controllable thickness of barium ferrite formation outside the nuclear, and shell thickness is adjustable in 10～100nm scope.Coprecipitation process is with the urea precipitation agent; preparation process has: need not barium titanate is carried out any surface modification; barium ferrite (ferromegnetism shell) controllable thickness; shell coats complete to nuclear; there is not independently shell particle existence in the product, with low cost, easy and simple to handle; equipment is simple, and is widely applicable and be suitable for the advantage of large-scale production.
Technical scheme of the present invention is as follows:
Ferroelectric-ferromagnetic multifunctional composite powder body material of the present invention is a kind of powder body material with nucleocapsid structure, and its nuclear is barium titanate, and nuclear is outer to be the ferromegnetism shell that constitutes with barium ferrite.The particle diameter of barium carbonate powder is in the scope of 0.05～2 μ m.
The present invention adopts even co-precipitation out-phase coating technology to prepare the multi-functional powder body material of nucleocapsid structure, and the preparation method utilizes the urea precipitation agent to decompose under the certain temperature condition to produce OH
-And CO
3 2-, improving the pH value of solution slowly, raising degree of supersaturation progressively makes GOLD FROM PLATING SOLUTION belong to ion generation precipitin reaction.Experiment conditions such as concentration by adjusting solution metal ionic concentration, urea and temperature of reaction, control precipitated metal thing is also grown with the mode forming core of out-phase forming core on the surface of ferroelectric powder, thereby realize of the coating of barium ferrite precursor, obtain ferroelectric-ferromagnetic core-shell particles precursor (hereinafter to be referred as precursor) barium carbonate powder; The precursor that obtains is placed under 800～1100 ℃ of conditions again and calcine 0.5～8h, the coating layer in the precursor is transformed into barium ferrite, thereby has obtained multi-functional compound barium titanate-barium ferrite composite powder material (hereinafter to be referred as core-shell material).
Preparation process of the present invention may further comprise the steps:
(1) the cleaning oil removing of barium carbonate powder: the certain volume barium carbonate powder is placed deionized water, and supersound process 10～30 minutes will be cleaned barium titanate later afterwards and be filtered collection; To place dehydrated alcohol through washed with de-ionized water barium titanate later, supersound process 10～40 minutes is filtered it afterwards and is collected; To place vacuum drying oven to dry in 50～80 ℃ of conditions through the barium titanate after the above-mentioned cleaning oil removing process, it be stand-by to obtain product;
(2) reaction soln configuration: according to stoichiometric ratio metal-salt is dissolved in the deionized water in the finite concentration ratio, treats to dissolve fully the back and in solution, add an amount of precipitation agent and tensio-active agent.Wherein the mol ratio of metal ion total amount and urea is 1: 20～200, and surfactant concentration is 0.05～0.8wt%;
Wherein, the metal-salt in the reaction soln is iron nitrate, nitrate of baryta, and the stoichiometric ratio of the shell that its volumetric molar concentration coats as required is configured, and the metal ion total mol concentration is 0.0001～0.08mol/L in the reaction soln, preferred 0.001～0.01; Precipitation agent is a urea in the reaction soln, and the volumetric molar concentration in reaction soln is 0.08～2.5mol/L, preferred 0.4～2.0mol/L; Tensio-active agent is one or both in polyvinylpyrrolidone, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, the polyvinyl alcohol, surfactant concentrations accounts for the mass percent definition that is coated barium carbonate powder of adding according to it in the reaction soln, its concentration is 0.05～0.8wt%, preferred 0.1～0.3wt%.
(3) precursor preparation: get and join in the reaction soln that obtains by step (2) in right amount through the barium titanate that cleans after the oil removing, supersound process is after 30～60 minutes under the room temperature condition, reaction soln is placed encloses container, under agitation condition, be incubated 1～48h again in 60～120 ℃.
Wherein, the adding concentration of barium titanate ferroelectric powder is 0.1～10g/L, preferred 1～5g/L;
(4) ageing: after treating that step (3) finishes,, and leave standstill 1～24h with reaction unit naturally cooling at ambient temperature.
(5) collect precursor: after treating that step (4) finishes, with the centrifugation under the 6000rpm condition of resulting product, remove and add ultrapure water again after the supernatant liquor and disperse again, centrifugal again, use earlier deionized water, repeat said process three times with dehydrated alcohol again, the precursor that cleans after separating is put into vacuum drying oven, at 50～80 ℃ of dry 12h.
(6) preparation barium titanate-barium ferrite composite granule: the precursor that step (5) makes is put into retort furnace,, obtain having the barium titanate-barium ferrite composite powder material of nucleocapsid structure at 600～1100 ℃ of calcining 0.5～8h.
In step of the present invention (1), the barium carbonate powder that is adopted can obtain by mechanical ball milling, sol-gel method, coprecipitation method and Hydrothermal Preparation.Referring to 1.Hu MZC, Payzant EA, Rawn CJ, Miller GA, " Homogeneous (co) precipitation of inorganic salts for synthesis of monodispersed barium titanate particles ", Journal of Materials Science 35 (2000) 2927-2936; 2.Burtrand Lee, Jianping Zhang, " Preparation, structure evolution and dielectric properties of BaTiO
3Thin films and powders by an aqueous sol-gel process ", Thin Solid Films 388 (2001) 107-113; 3. Chinese patent CN1275117; 4. open sword light, Zhang Mingfu, Han Jiecai, He Xiaodong, Du Shanyi, " high-energy ball milling method prepares the crystallization process of nano barium phthalate ", piezoelectricity and acousto-optic, 200123 (5).
The invention has the advantages that: the barium titanate-barium ferrite composite granule of the present invention's preparation is the ferroelectric-ferromagnetic multifunctional composite powder body of nucleocapsid structure, its ferroelectric and ferromagnetic property can be regulated and control easily within the specific limits, and powder has stronger magneto-electric coupled coefficient.Deposition process is precipitation agent with urea; prepared matrix material coats complete; product is single; no independent shell particle exists; coating thickness is adjustable in 10～100nm scope, need not barium carbonate powder is carried out surface modification, and the preparation method is simple; need not the main equipment instrument, be applicable to large-scale production.
Description of drawings
Fig. 1 is the prepared precursor of embodiment 1 and the TEM (a is a precursor, and b is a core-shell particles) of core-shell particles;
Fig. 2 is the XRD spectra (a barium titanate, b precursor, c core-shell particles) for prepared barium titanate, precursor and core-shell particles of embodiment 1;
Fig. 3 is the magnetic hysteresis loop for the prepared core-shell particles of embodiment 1.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Embodiment 1
Take by weighing an amount of Fe (NO
3)
39H
2O, Ba (NO
3)
2Be dissolved in urea and make three's volumetric molar concentration be respectively 0.006mol/L, 0.0005mol/L, 0.8mol/L in the deionized water, take by weighing 0.5g and remove japanned barium carbonate powder through cleaning, join in the above-mentioned reaction soln of 200ml, the polyvinylpyrrolidone that adds 3wt% simultaneously is as dispersion agent.After 30 minutes, place encloses container to react under agitation condition through supersound process above-mentioned solution, temperature of reaction is 100 ℃, and the reaction times is 12 hours; The reaction finish after with the suspension centrifugation under the 6000rpm condition that obtains, remove and add ultrapure water again after the supernatant liquor and disperse again, centrifugal again, use earlier deionized water, repeat said process respectively three times with dehydrated alcohol again, the coating precursor that cleans after separating is put into vacuum drying oven dry 12h under 80 ℃ of conditions; Dried coating precursor is put into retort furnace, under 1100 ℃ of conditions, calcine 2h, obtain barium ferrite (BaFe
12O
9) coating barium titanate (BaTiO
3) nucleocapsid structure ferroelectric-ferromagnetic composite powder material.Its barium ferrite coating layer mean thickness is 12nm.TEM photo, XRD and the magnetic hysteresis loop of precursor and core-shell particles are respectively as Fig. 1, Fig. 2 and shown in Figure 3 under this condition.
Embodiment 2
Take by weighing an amount of Fe (NO
3)
39H
2O, Ba (NO
3)
2Be dissolved in urea and make three's volumetric molar concentration be respectively 0.006mol/L, 0.0005mol/L, 0.8mol/L in the deionized water, take by weighing 0.1g and remove japanned barium carbonate powder through cleaning, join in the above-mentioned reaction soln of 200ml, the polyvinylpyrrolidone that adds 3wt% simultaneously is as dispersion agent.After 30 minutes, place encloses container to react under agitation condition through supersound process above-mentioned solution, temperature of reaction is 100 ℃, and the reaction times is 12 hours; The reaction finish after with the suspension centrifugation under the 6000rpm condition that obtains, remove and add ultrapure water again after the supernatant liquor and disperse again, centrifugal again, use earlier deionized water, repeat said process respectively three times with dehydrated alcohol again, the coating precursor that cleans after separating is put into vacuum drying oven dry 12h under 80 ℃ of conditions; Dried coating precursor is put into retort furnace, under 1100 ℃ of conditions, calcine 2h, obtain barium ferrite (BaFe
12O
9) coating barium titanate (BaTiO
3) nucleocapsid structure ferroelectric-ferromagnetic composite powder material.Its barium ferrite coating layer mean thickness is 23nm.
Embodiment 3
Take by weighing an amount of Fe (NO
3)
39H
2O, Ba (NO
3)
2Be dissolved in urea and make three's volumetric molar concentration be respectively 0.024mol/L, 0.002mol/L, 0.8mol/L in the deionized water, take by weighing 0.5g and remove japanned barium carbonate powder through cleaning, join in the above-mentioned reaction soln of 200ml, the polyvinylpyrrolidone that adds 3wt% simultaneously is as dispersion agent.After 30 minutes, place encloses container to react under agitation condition through supersound process above-mentioned solution, temperature of reaction is 90 ℃, and the reaction times is 24 hours; The reaction finish after with the suspension centrifugation under the 6000rpm condition that obtains, remove and add ultrapure water again after the supernatant liquor and disperse again, centrifugal again, use earlier deionized water, repeat said process respectively three times with dehydrated alcohol again, the coating precursor that cleans after separating is put into vacuum drying oven dry 12h under 80 ℃ of conditions; Dried coating precursor is put into retort furnace, under 800 ℃ of conditions, calcine 2h, obtain barium ferrite (BaFe
12O
9) coating barium titanate (BaTiO
3) nucleocapsid structure ferroelectric-ferromagnetic composite powder material.
Claims (4)
1. nucleocapsid structure barium titanate-barium ferrite composite powder material, it is characterized in that, this material is the ferroelectric-ferromagnetic multifunctional composite powder body material with nucleocapsid structure, and its nuclear is ferroelectric powder material barium titanate, is the ferromegnetism shell with the controllable thickness of barium ferrite formation outside the nuclear.
2. the preparation method of nucleocapsid structure barium titanate as claimed in claim 1-barium ferrite composite powder material is characterized in that concrete steps are as follows:
(1) the cleaning oil removing of barium carbonate powder: the certain volume barium carbonate powder is placed deionized water, and supersound process 10～30 minutes will be cleaned barium titanate later afterwards and be filtered collection; To place dehydrated alcohol through washed with de-ionized water barium titanate later, supersound process 10～40 minutes is filtered it afterwards and is collected; To place vacuum drying oven to dry in 50～80 ℃ of conditions through the barium titanate after the above-mentioned cleaning oil removing process, it be stand-by to obtain product;
(2) reaction soln preparation: according to stoichiometric ratio metal-salt is dissolved in the deionized water in the finite concentration ratio, treats to dissolve fully the back and in solution, add an amount of precipitation agent and tensio-active agent;
(3) precursor preparation: get an amount of barium titanate that cleans after the oil removing through step (1) and join in the reaction soln that obtains by step (2), supersound process is after 30～60 minutes under the room temperature condition, reaction soln is placed encloses container, under agitation condition, be incubated 1～48h again in 60～120 ℃;
(4) ageing: after treating that step (3) finishes,, and leave standstill 1～24h with reaction unit naturally cooling at ambient temperature;
(5) collect precursor: after treating that step (4) finishes, with the centrifugation under the 6000rpm condition of resulting product, remove and add ultrapure water again after the supernatant liquor and disperse again, centrifugal again, use earlier deionized water, repeat said process three times with dehydrated alcohol again, the precursor that cleans after separating is put into vacuum drying oven, at 50～80 ℃ of dry 12h;
(6) preparation barium titanate-barium ferrite composite granule: the precursor that step (5) makes is put into retort furnace,, obtain having the barium titanate-barium ferrite composite powder material of nucleocapsid structure at 600～1100 ℃ of calcining 0.5～8h.
3. as the described reaction soln preparation of claim 2 step (2), it is characterized in that, solution metal salt is iron nitrate, nitrate of baryta, the stoichiometric ratio of the shell that its volumetric molar concentration coats as required is configured, the metal ion total mol concentration is 0.0001～0.08mol/L in the reaction soln, preferred 0.001～0.01; Precipitation agent is a urea in the reaction soln, and the volumetric molar concentration in reaction soln is 0.08～2.5mol/L, preferred 0.4～2.0mol/L; Tensio-active agent is one or both in polyvinylpyrrolidone, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, the polyvinyl alcohol, surfactant concentrations accounts for the mass percent definition that is coated ferroelectric powder of adding according to it in the reaction soln, its concentration is 0.05～0.8wt%, preferred 0.1～0.3wt%.
4. as the described precursor preparation of claim 2 step (3), it is characterized in that the adding concentration of barium titanate ferroelectric powder is 0.1～10g/L, preferred 1～5g/L.
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