CN106431391A - Method for preparing Bi4Ti(3-x)VxO12 powder - Google Patents

Method for preparing Bi4Ti(3-x)VxO12 powder Download PDF

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CN106431391A
CN106431391A CN201610820915.6A CN201610820915A CN106431391A CN 106431391 A CN106431391 A CN 106431391A CN 201610820915 A CN201610820915 A CN 201610820915A CN 106431391 A CN106431391 A CN 106431391A
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powder
beaker
ethylene glycol
certain amount
solution
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夏傲
于婉茹
谈国强
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • 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
    • C04B35/624—Sol-gel processing
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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    • 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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
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    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm

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Abstract

A method for preparing Bi4Ti(3-x)VxO12 powder comprises the following steps: a certain amount of Bi(NO3)3.5H2O is weighed and fed into a first beaker, ethylene glycol is added slowly to the beaker, and the beaker is left to stand for a period of time to enable Bi(NO3)3.5H2O to be dissolved in the ethylene glycol completely; then a certain amount of Ti(OC4H9)4 and a certain amount of V2O5 are weighed respectively and fed into a second beaker, ethylene glycol and glacial acetic acid are added to the second beaker, the materials are stirred uniformly, and a brown solution is obtained; the solution in the first beaker is added to the second beaker slowly, the mixture is stirred magnetically for 3-4 h, and faint yellow transparent sol is obtained; the beaker filled with the mixed solution is placed in a drying oven at 80 DEG C and left to stand for 24 h, and white gel is obtained; the white gel product is placed into the drying oven at 90 DEG C, completely dried and ground into powder; the dry gel powder is calcined at 550-650 DEG C for 1-2 h, and the Bi4Ti(3-x)VxO12 powder is obtained. The method has the characteristics that the powder particles are fine and uniform, and the average size is smaller than 100 nanometers.

Description

One kind prepares Bi4Ti3-xVxO12The method of powder
Technical field
The present invention relates to field of functional materials, prepare Bi particularly to one kind4Ti3-xVxO12The method of powder.
Background technology
Bismuth titanates Bi4Ti3O12Belong to laminated perovskite sections electric material, due to this special layer structure so that titanium Sour bismuth has excellent performance：Low-k, high-curie temperature, electromechanical coupling factor anisotropy substantially, piezoelectricity respectively to The opposite sex substantially, high dielectric strength, low ageing rate, high resistivity, big dielectric breakdown strength, low sintering temperature.Therefore, bismuth layer Shape bismuth titanate ceramics is that one kind is particularly suitable for high temperature, the piezoelectric that high frequency field uses.
It has been found that Doped ions change material to a great extent in the research to the doping vario-property of ferroelectric material Structure, thus causing the change of material ferroelectric properties.To bismuth laminated Bi4Ti3O12Doping vario-property be mainly A position, B Adulterating substitution in position and A/B position simultaneously, selects suitable doped chemical and find suitable component and can substantially improve Bi4Ti3O12The properties of material.
At present, Bi4Ti3O12Research be concentrated mainly on Bi4Ti3O12The preparation of ferroelectric thin film and the exploitation of ferroelectric memory, Multiple advanced technology preparation Bi are developed4Ti3O12Film, mainly has：Organometallic solutions sedimentation, Metal Organic Chemical Vapor Sedimentation, sol-gel process, pulsed laser deposition, magnetron sputtering method etc., be mainly used in permanent memory device and high density with Machine memory, piezoelectricity and electro-optical device, the aspect such as real time holography.Relatively fewer, bismuth titanates is reported in the preparation of bismuth titanate powder Raw powder's production technology mainly has solid phase method, coprecipitation, hydro-thermal method.
But above-mentioned prior art has the appearance of high temperature dephasign in preparation process, the purity of product is relatively low, and the group of powder Poly- heavier；In preparation process, skewness, valence state are unstable in the material for doped chemical, and material property is relatively low.
Content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, it is an object of the invention to provide one kind prepares Bi4Ti3-xVxO12Powder The method of body, has prepared Bi using sol-gel process4Ti3-xVxO12Powder, gained powder crystalline phase develops complete, purity height； Grain morphology rule, average-size are less than 100 nanometers.
For achieving the above object, the technical solution used in the present invention is：
A kind of method preparing Bi4Ti3-xVxO12 powder, comprises the following steps：
Step 1：Weigh a certain amount of Bi (NO3)3·5H2O is placed in No. 1 beaker, is slowly added to ethylene glycol thereto, quiet Put and make Bi (NO for a period of time3)3·5H2O is dissolved completely in ethylene glycol；
Step 2：Weigh a certain amount of Ti (OC respectively4H9)4And V2O5Be placed in No. 2 beakers, be added thereto to ethylene glycol and Glacial acetic acid, the volume ratio of described ethylene glycol and glacial acetic acid is (8～10) 1, is uniformly mixing to obtain brown solution；
Step 3：Solution in No. 1 beaker is slowly added in No. 2 beakers, magnetic agitation, after 3～4 hours, obtains yellowish Color vitreosol；Wherein, Bi3+The concentration of ion is 0.4～1.2mol/L, Bi3+、Ti4+、V5+The mol ratio of ion is 4 3-x X, wherein x=0.01-0.10；
Step 4：Mixed solution beaker in step 3 is put in 80 DEG C of baking oven, obtains white after placing 24h solidifying Glue product；
Step 5：White gels product in step 4 is put in 90 DEG C of baking ovens, after being completely dried, grinds to form powder；
Step 6：The dry gel powder grinding to form powder in step 5 is calcined 1～2h at 550～650 DEG C, obtains Bi4Ti3- xVxO12Powder.
Beneficial effects of the present invention：
The present invention adopts sol-gel process, has prepared Bi4Ti3-xVxO12Powder, process is simple, efficiency high, gained powder The crystalline phase of body is developed, and purity is high, V5+Ion is mixed with Bi4Ti3O12In lattice, and in Bi4Ti3O12It is evenly distributed in powder, Powder granule is tiny, uniform, average-size is less than 100 nanometers.Sol-gel process advantage is：Reaction raw materials are on a molecular scale Mix, calcining heat is low, thus avoiding the appearance of high temperature dephasign, the purity of product is higher, and the reunion of powder is light；This Outer when preparing doping type powder using sol-gel process, doped chemical is evenly distributed in the material, valence stability, is conducive to material The raising of material performance.
Brief description
Fig. 1 is the Bi of present invention preparation4Ti2.97V0.03O12Powder XRD spectrum.
Fig. 2 is the Bi of present invention preparation4Ti2.97V0.03O12The SEM figure of powder.
Fig. 3 is the Bi of present invention preparation4Ti2.97V0.03O12The EDS collection of illustrative plates of powder.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is described in further detail.
Embodiment one；
Step 1：Weigh the Bi (NO of 0.016mol3)3·5H2O is placed in No. 1 beaker, is slowly added to 10mL second two thereto Alcohol, standing a period of time makes Bi (NO3)3·5H2O is dissolved completely in ethylene glycol；
Step 2：Weigh 0.012mol Ti (OC respectively4H9)4With 2 × 10-5mol V2O5It is placed in No. 2 beakers, thereto Add 9mL ethylene glycol and 1mL glacial acetic acid, be uniformly mixing to obtain brown solution；
Step 3：Solution in No. 1 beaker is slowly added in No. 2 beakers, magnetic agitation, after 3 hours, obtains faint yellow Bright colloidal sol；Wherein, Bi3+The concentration of ion is 0.4mol/L, Bi3+、Ti4+、V5+The mol ratio of ion is 4 2.99 0.01；
Step 4：Mixed solution beaker in step 3 is put in 80 DEG C of baking oven, obtains white after placing 24h solidifying Glue product；
Step 5：White gels product is put in 90 DEG C of baking ovens, after being completely dried, grinds to form powder；
Step 6：The dry gel powder grinding to form powder in step 5 is calcined 2h at 550 DEG C, obtains Bi4Ti2.99V0.01O12Powder Body.
Embodiment two
Step 1：Weigh the Bi (NO of 0.032mol3)3·5H2O is placed in No. 1 beaker, is slowly added to 10mL second two thereto Alcohol, standing a period of time makes Bi (NO3)3·5H2O is dissolved completely in ethylene glycol；
Step 2：Weigh 0.024mol Ti (OC respectively4H9)4With 1.2 × 10-4mol V2O5It is placed in No. 2 beakers, Xiang Qi Middle addition 9mL ethylene glycol and 1mL glacial acetic acid, are uniformly mixing to obtain brown solution；
Step 3：Solution in No. 1 beaker is slowly added in No. 2 beakers, magnetic agitation, after 3 hours, obtains faint yellow Bright colloidal sol；Wherein, Bi3+The concentration of ion is 0.8mol/L, Bi3+、Ti4+、V5+The mol ratio of ion is 4 2.97 0.03；
Step 4：Mixed solution beaker in step 3 is put in 80 DEG C of baking oven, obtains white after placing 24h solidifying Glue product；
Step 5：White gels product is put in 90 DEG C of baking ovens, after being completely dried, grinds to form powder；
Step 6：The dry gel powder grinding to form powder in step 5 is calcined 1.5h at 600 DEG C, obtains Bi4Ti2.97V0.03O12 Powder.
Embodiment three
Step 1：Weigh the Bi (NO of 0.048mol3)3·5H2O is placed in No. 1 beaker, is slowly added to 10mL second two thereto Alcohol, standing a period of time makes Bi (NO3)3·5H2O is dissolved completely in ethylene glycol；
Step 2：Weigh 0.035mol Ti (OC respectively4H9)4With 6.0 × 10-4mol V2O5It is placed in No. 2 beakers, Xiang Qi Middle addition 9mL ethylene glycol and 1mL glacial acetic acid, are uniformly mixing to obtain brown solution；
Step 3：Solution in No. 1 beaker is slowly added in No. 2 beakers, magnetic agitation, after 3 hours, obtains faint yellow Bright colloidal sol；Wherein, Bi3+The concentration of ion is 1.2mol/L, Bi3+、Ti4+、V5+The mol ratio of ion is 4 2.90 0.10；
Step 4：Mixed solution beaker in step 3 is put in 80 DEG C of baking oven, obtains white after placing 24h solidifying Glue product；
Step 5：White gels product is put in 90 DEG C of baking ovens, after being completely dried, grinds to form powder；
Step 6：The dry gel powder grinding to form powder in step 5 is calcined 1h at 650 DEG C, obtains Bi4Ti2.9V0.1O12Powder Body.
Fit like a glove with the standard card NO.35-0795 in PDF database in Fig. 1, illustrate that the crystalline phase of powder consists of Bi4Ti3O12, the other impurities containing V element, V is described in figure5+Ion comes into Bi4Ti3O12Lattice in, In addition the peak type at X-ray diffraction peak is sharp, peak intensity is higher, illustrates that powder crystal formation physically well develops.
In Fig. 2, preferably, pattern is relatively regular, and average particle size particle size is less than 100nm for visible powder granule dispersiveness.
V element is contained in the component of visible composition powder, the test result of EDS demonstrates XRD's further in Fig. 3 Result.

Claims (1)

1. a kind of method preparing Bi4Ti3-xVxO12 powder is it is characterised in that comprise the following steps：
Step 1：Weigh a certain amount of Bi (NO3)3·5H2O is placed in No. 1 beaker, is slowly added to ethylene glycol thereto, stands one The section time makes Bi (NO3)3·5H2O is dissolved completely in ethylene glycol；
Step 2：Weigh a certain amount of Ti (OC respectively4H9)4And V2O5It is placed in No. 2 beakers, be added thereto to ethylene glycol and ice second The volume ratio of acid, ethylene glycol and glacial acetic acid is (8～10) 1, is uniformly mixing to obtain brown solution；
Step 3：Solution in No. 1 beaker is slowly added in No. 2 beakers, magnetic agitation, after 3～4 hours, obtains faint yellow Bright colloidal sol；Wherein, Bi3+The concentration of ion is 0.4～1.2mol/L, Bi3+、Ti4+、V5+The mol ratio of ion is 4 3-x x, x= 0.01-0.10；
Step 4：Mixed solution beaker in step 3 is put in 80 DEG C of baking oven, obtains white gels after placing 24h and produce Thing；
Step 5：White gels product in step 4 is put in 90 DEG C of baking ovens, after being completely dried, grinds to form powder；
Step 6：The dry gel powder grinding to form powder in step 5 is calcined 1～2h at 550～650 DEG C, obtains Bi4Ti3-xVxO12Powder Body.
CN201610820915.6A 2016-09-13 2016-09-13 Method for preparing Bi4Ti(3-x)VxO12 powder Pending CN106431391A (en)

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