CN105923650B - One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder - Google Patents

One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder Download PDF

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CN105923650B
CN105923650B CN201610247803.6A CN201610247803A CN105923650B CN 105923650 B CN105923650 B CN 105923650B CN 201610247803 A CN201610247803 A CN 201610247803A CN 105923650 B CN105923650 B CN 105923650B
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powder
nanometer
precipitation
white precipitate
block
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CN105923650A (en
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曹丽云
罗艺佳
周磊
黄剑锋
吴建鹏
闫婧文
李瑞梓
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

Nanometer Bi is prepared using precipitation calcination method the invention discloses one kind2Zr2O7The method of powder, belongs to technical field of material.Comprise the following steps：1) Bi (NO are taken3)3·5H2O and Zr (NO3)4·5H2O；2) Bi (NO are dissolved with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O, then two kinds of solution for dissolving to obtain respectively are mixed, precursor liquid A is made；3) adjust precursor liquid A pH value, stir, obtain precipitated liquid B, filter, white precipitate C is made；4) after white precipitate C is dried, block is made, block is fully ground, obtains powder D；5) powder D is heat-treated, nanometer Bi is made2Zr2O7Powder.Not only technique is simple for this method, easy to operate, and is more easy in precipitation process to realize that atom level uniformly mixes, and may advantageously facilitate the low temperature synthesis of material, short preparation period, cost is low, therefore has vast potential for future development.The Bi of size uniform can be made through the inventive method2Zr2O7Nano material, and particle diameter is small, better crystallinity degree.

Description

One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder
Technical field
The invention belongs to technical field of material, and in particular to one kind prepares nanometer Bi using precipitation calcination method2Zr2O7 The method of powder.
Background technology
Zirconic acid bismuth (Bi2Zr2O7) belong to pyrochlore-type composite oxide of metal.It is a kind of with ionic conductivity, ferroelectricity The inorganic composite material of the multiple performances such as ferromagnetic, photocatalytic.[Zeng Weiwei, Xiao Caimei, Chen Hong rosy clouds pyrochlore-types are compound The preparation of oxide and its photocatalysis performance [J] chemical intermediates, 2011, (4)：32-35.].Typical pyrochlore type structure Formula be A2B2O7, (wherein A, B are respectively+3 valencys and+4 valency cations), belong to a cube center of area crystallographic system, belong to Fd3m spaces Group, this structure may be considered by the cation (A of two kinds of different radiis3+、B4+) and 1/8 anion vacancy composition fluorite Type structure [Erickson E E, Gray D, Taylor K, et al.Synthesis, structure and dielectric characterization of Ln2Ti2-2xM2xO7(Ln=Gd, Er；M=Zr, Sn, Si) [J] .Materials Research Bulletin,2002,37:2077-2083].As pyrochlore type multiple oxide, zirconic acid bismuth (Bi2Zr2O7) because its have compared with Wide energy gap (2.59~2.9eV), it is a kind of visible-light-responsive photocatalyst with development potentiality.
At present, the preparation method of pyrochlore-type composite has vapor phase method, solid phase method and liquid phase method.And for zirconic acid bismuth (Bi2Zr2O7) research be scarcely out of swaddling-clothes, relevant its preparation method, be also rarely reported.Precipitation calcination method belongs to solid phase method One kind.Such as Deyong Wu [D.Wu, T.He, J.Xia, Y.Tan. Preparation and photocatalytic properties of Bi2Zr2O7photocatalyst[J].Material Letters,156(2015):195-197.] with Bi(NO3)3·5H2O and Zr (NO3)4·5H2O is raw material, and the first stage uses hydro-thermal method, presoma sediment is made, through washing Wash, dry, grind, calcined 4 hours under the conditions of 600 DEG C, Bi is made2Zr2O7Target product.But this method preparation process is complicated, Power consumption is high, cycle length.
The content of the invention
The defects of in order to overcome above-mentioned prior art to exist, it is an object of the invention to provide one kind using precipitation calcination method Prepare nanometer Bi2Zr2O7The method of powder, this method operating process is simple, and the cycle is short, and power consumption is low.
The present invention is to be achieved through the following technical solutions：
One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder, comprises the following steps：
1) Bi (NO are pressed3)3·5H2O：Zr(NO3)4·5H2O=1:1 mol ratio, take Bi (NO3)3·5H2O and Zr (NO3)4·5H2O；
2) Bi (NO are dissolved with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O, then will be molten respectively Two kinds of solution mixing that solution obtains, is made Bi3+Concentration is 0.025~0.05mol/L precursor liquid A；；
3) adjust precursor liquid A pH value to 4.0~10.0, stir, obtain precipitated liquid B, filter, be made white Color precipitate C；
4) after white precipitate C is dried, block is made, block is fully ground, obtains powder D；
5) by powder D at 500~800 DEG C, 2~10h is heat-treated, nanometer Bi is made2Zr2O7Powder.
Step 2) is that precursor liquid A is placed on magnetic stirring apparatus, and pH value, and not stopping pregnancy during regulation are adjusted with concentrated ammonia liquor Raw white precipitate.
The time that step 2) stirs is 2~4h.
Step 4) the drying is that white precipitate C is placed in thermostatic drying chamber, is dried at 60~100 DEG C.
Step 4) is described to be fully ground, and is that block is placed in agate mortar, is fully ground 5~20min.
Step 5) is that powder D is put into crucible, is subsequently placed in Muffle furnace and is heat-treated.
Compared with prior art, the present invention has technique effect beneficial below：
The present invention prepares Bi using precipitation calcination method2Zr2O7Nano material, using the precipitation method by adding corresponding precipitation Agent, two kinds of precipitations can be made slowly uniformly to be separated out from solution, then be calcined by the later stage, obtain the target product of size uniform. Not only technique is simple for this method, easy to operate, and is more easy in precipitation process to realize that atom level uniformly mixes, and may advantageously facilitate The low temperature synthesis of material, short preparation period, cost is low, therefore has vast potential for future development.It can be made through the inventive method The Bi of size uniform2Zr2O7Nano material, and particle diameter is small, better crystallinity degree.
Brief description of the drawings
Fig. 1 is present invention Bi obtained under conditions of example 32Zr2O7X-ray diffraction (XRD) collection of illustrative plates；
Fig. 2 is present invention Bi prepared under the conditions of example 32Zr2O7ESEM (SEM) photo of nano material； Wherein, (a) is Bi under 100,000 enlargement ratios2Zr2O7The SEM figures of nano material；(b) it is Bi under 180,000 enlargement ratios2Zr2O7Receive The SEM figures of rice material.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and It is not to limit.
Embodiment 1
One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder, comprises the following steps：
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi respectively (NO3)3·5H2O and Zr (NO3)4·5H2O dissolves Bi (NO in beaker, with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O.Both are mixed after stirring the regular hour respectively, prepares Bi3+Concentration is 0.025mol/L precursor liquid A.
2) gained precursor liquid A is placed on magnetic stirring apparatus, concentrated ammonia liquor is slowly added dropwise and adjusts its pH=10.00, is adjusting During constantly have a white precipitate generation, stir 2h, it is sufficiently mixed uniformly, acquisition precipitated liquid B.
3) precipitation in precipitated liquid B is separated into wash-off with impurity using the means of suction filtration, obtains white precipitate C.
4) the white precipitate C of gained is placed in thermostatic drying chamber, control temperature dries 12h at 60 DEG C.It will be obtained after drying The block obtained, which is placed in agate mortar, is fully ground 10min, obtains powder D.
5) the powder D of acquisition is put into crucible, be placed in Muffle furnace, at a temperature of 500 DEG C, be heat-treated 8h, it is final Obtain the Bi of nano-scale2Zr2O7Powder.
Embodiment 2
One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder, comprises the following steps：
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi respectively (NO3)3·5H2O and Zr (NO3)4·5H2O dissolves Bi (NO in beaker, with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O.Both are mixed after stirring the regular hour respectively, prepares Bi3+Concentration is 0.03mol/L precursor liquid A.
2) gained precursor liquid A is placed on magnetic stirring apparatus, concentrated ammonia liquor is slowly added dropwise and adjusts its pH=10.00, is adjusting During constantly have a white precipitate generation, stir 2h, it is sufficiently mixed uniformly, acquisition precipitated liquid B.
3) precipitation in precipitated liquid B is separated into wash-off with impurity using the means of suction filtration, obtains white precipitate C.
4) the white precipitate C of gained is placed in thermostatic drying chamber, control temperature dries 10h at 70 DEG C.It will be obtained after drying The block obtained, which is placed in agate mortar, is fully ground 15min, obtains powder D.
5) the powder D of acquisition is put into crucible, be placed in Muffle furnace, at a temperature of 600 DEG C, be heat-treated 6h, it is final Obtain the Bi of nano-scale2Zr2O7Powder.
Embodiment 3
One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder, comprises the following steps：
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi respectively (NO3)3·5H2O and Zr (NO3)4·5H2O dissolves Bi (NO in beaker, with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O.Both are mixed after stirring the regular hour respectively, prepares Bi3+Concentration is 0.05mol/L precursor liquid A.
2) gained precursor liquid A is placed on magnetic stirring apparatus, concentrated ammonia liquor is slowly added dropwise and adjusts its pH=7.00, was adjusting Constantly there is white precipitate generation in journey, stir 3h, it is sufficiently mixed uniformly, obtain precipitated liquid B.
3) precipitation in precipitated liquid B is separated into wash-off with impurity using the means of suction filtration, obtains white precipitate C.
4) the white precipitate C of gained is placed in thermostatic drying chamber, control temperature dries 8h at 80 DEG C.It will be obtained after drying The block obtained, which is placed in agate mortar, is fully ground 5min, obtains powder D.
5) the powder D of acquisition is put into crucible, be placed in Muffle furnace, at a temperature of 600 DEG C, be heat-treated 10h, it is final to be It can obtain the Bi of nano-scale2Zr2O7Powder.
Bi made from the present embodiment2Zr2O7X-ray diffraction (XRD) collection of illustrative plates of nano material, can from figure referring to Fig. 1 Go out, the present invention can prepare the Bi of pure phase under cryogenic2Zr2O7。
Referring to Fig. 2, wherein, (a) is Bi under 100,000 enlargement ratios2Zr2O7The SEM figures of nano material；(b) it is 180,000 amplifications Bi under multiplying power2Zr2O7The SEM figures of nano material.Figure it is seen that Bi is prepared using precipitation calcination method2Zr2O7Particle size Between 20~30nm.
Embodiment 4
One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder, comprises the following steps：
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi respectively (NO3)3·5H2O and Zr (NO3)4·5H2O dissolves Bi (NO in beaker, with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O.Both are mixed after stirring the regular hour respectively, prepares Bi3+Concentration is 0.025mol/L precursor liquid A.
2) gained precursor liquid A is placed on magnetic stirring apparatus, concentrated ammonia liquor is slowly added dropwise and adjusts its pH=7.00, was adjusting Constantly there is white precipitate generation in journey, stir 3h, it is sufficiently mixed uniformly, obtain precipitated liquid B.
3) precipitation in precipitated liquid B is separated into wash-off with impurity using the means of suction filtration, obtains white precipitate C.
4) the white precipitate C of gained is placed in thermostatic drying chamber, control temperature dries 7h at 90 DEG C.It will be obtained after drying The block obtained, which is placed in agate mortar, is fully ground 20min, obtains powder D.
5) the powder D of acquisition is put into crucible, be placed in Muffle furnace, at a temperature of 700 DEG C, be heat-treated 4h, it is final Obtain the Bi of nano-scale2Zr2O7Powder.
Embodiment 5
One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder, comprises the following steps：
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi respectively (NO3)3·5H2O and Zr (NO3)4·5H2O dissolves Bi (NO in beaker, with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O.Both are mixed after stirring the regular hour respectively, prepares Bi3+Concentration is 0.04mol/L precursor liquid A.
2) gained precursor liquid A is placed on magnetic stirring apparatus, concentrated ammonia liquor is slowly added dropwise and adjusts its pH=4.00, was adjusting Constantly there is white precipitate generation in journey, stir 4h, it is sufficiently mixed uniformly, obtain precipitated liquid B.
3) precipitation in precipitated liquid B is separated into wash-off with impurity using the means of suction filtration, obtains white precipitate C.
4) the white precipitate C of gained is placed in thermostatic drying chamber, control temperature dries 5h at 100 DEG C.It will be obtained after drying The block obtained, which is placed in agate mortar, is fully ground 15min, obtains powder D.
5) the powder D of acquisition is put into crucible, be placed in Muffle furnace, at a temperature of 800 DEG C, be heat-treated 2h, it is final Obtain the Bi of nano-scale2Zr2O7Powder.
In summary, the present invention provides that a kind of building-up process is simple, synthetic method-precipitation that the cycle is shorter, cost is low is forged Burning method prepares Bi2Zr2O7Nano material.Precipitation calcination method prepares the Bi of nano-scale2Zr2O7The advantage of powder is：Using heavy Shallow lake method can be such that two kinds of precipitations are slowly uniformly separated out from solution by adding corresponding precipitating reagent, then be calcined by the later stage, obtain Obtain the target product of size uniform.Not only technique is simple for this method, and is more easy in precipitation process to realize that atom level is uniformly mixed Close, may advantageously facilitate the low temperature synthesis of material.

Claims (3)

1. one kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder, it is characterised in that comprise the steps of：
1) Bi (NO are pressed3)3·5H2O：Zr(NO3)4·5H2O=1:1 mol ratio, take Bi (NO3)3·5H2O and Zr (NO3)4· 5H2O；
2) Bi (NO are dissolved with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O, then it will dissolve respectively The two kinds of solution mixing arrived, is made Bi3+Concentration is 0.025~0.05mol/L precursor liquid A；
3) precursor liquid A is placed on magnetic stirring apparatus, adjusts pH value to 4.0~10.0 with concentrated ammonia liquor, be sufficiently stirred 2~4h, obtain To precipitated liquid B, filter, white precipitate C is made；
4) white precipitate C is placed in thermostatic drying chamber, at 60~100 DEG C, dries 5~12h, block is made, block is filled Divide grinding, obtain powder D；
5) by powder D at 500~700 DEG C, 4~10h is heat-treated, nanometer of the particle size between 20~30nm is made Bi2Zr2O7Powder.
2. according to claim 1 prepare nanometer Bi using precipitation calcination method2Zr2O7The method of powder, it is characterised in that Step 4) is described to be fully ground, and is that block is placed in agate mortar, is fully ground 5~20min.
3. according to claim 1 prepare nanometer Bi using precipitation calcination method2Zr2O7The method of powder, it is characterised in that Step 5) is that powder D is put into crucible, is subsequently placed in Muffle furnace and is heat-treated.
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