CN105692697A - Method for preparing nanometer Bi2Zr2O7 powder by sedimentation-calcination method assisted with molten salt method - Google Patents
Method for preparing nanometer Bi2Zr2O7 powder by sedimentation-calcination method assisted with molten salt method Download PDFInfo
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- C01G29/00—Compounds of bismuth
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a method for preparing nanometer Bi2Zr2O7 powder by sedimentation-calcination method assisted with a molten salt method, and belongs to the technical field of material preparation. The method includes steps of 1) taking Bi(NO3)3.5H2O and Zr (NO3)4.5H2O; 2) dissolving Bi(NO3)3.5H2O using concentrated nitric acid and Zr (NO3)4.5H2O using deionized water, mixing the two kinds of dissolved solutions to prepare precursor liquid A; 3) adjusting pH value of the precursor liquid, uniformly and sufficiently stirring to obtain sediment B, and filtering by suction to produce white sediment C; 4) drying the white sediment C to produce blocks, and grinding the blocks sufficiently to produce powder D; mixing the powder D with double salt composed of potassium nitrate and sodium nitrate, and using thermal treatment to produce nanometer Bi2Zr2O7. The method is simple in process, convenient to operate, short in preparation cycle and low in synthesis temperature and cost, and has wide development prospect. Bi2Zr2O7 nano materials produced by the method are uniform in size, small in grain size and excellent in crystallinity.
Description
Technical field
The invention belongs to technical field of material, be specifically related to a kind of employing and precipitate calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body。
Background technology
Zirconic acid bismuth (Bi2Zr2O7) belong to a cube center of area crystallographic system, belong to Fd3m space group, belong to pyrochlore type multiple oxide。The formula of typical pyrochlore type structure is A2B2O7, (wherein A, B respectively+3 valencys and+4 valency cationes), 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 [EricksonEE, GrayD, TaylorK, etal.Synthesis, StructureanddielectriccharacterizationofLn2Ti2-2xM2xO7(Ln=Gd, Er；M=Zr, Sn, Si) [J] .MaterialsResearchBulletin, 2002,37:2077 2083]。As pyrochlore type multiple oxide, zirconic acid bismuth (Bi2Zr2O7) because it has wider 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) understanding also in a kind of primary stage, relevant its preparation method, also rarely have report。Precipitation calcination method belongs to the one of solid phase method。Such as [D.Wu, T.He, J.Xia, Y.Tan.PreparationandphotocatalyticpropertiesofBi such as DeyongWu2Zr2O7Photocatalyst [J] .MaterialLetters, 156 (2015): 195-197.] with Bi (NO3)3·5H2O and Zr (NO3)4·5H2O is raw material, and the first stage adopts hydro-thermal method, prepares presoma precipitate, scrubbed, dry, grinding, calcines 4 hours, prepare Bi under 600 DEG C of conditions2Zr2O7Target product。But the method preparation process is complicated, and the cycle is long, synthesis temperature is high。
Summary of the invention
For the defect overcoming above-mentioned prior art to exist, it is an object of the invention to provide a kind of employing and precipitate calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, the method operating process is simple, and the cycle is short, and synthesis temperature is low。
The present invention is achieved through the following technical solutions:
A kind of employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, comprises the following steps:
1) by Bi (NO3)3·5H2O:Zr (NO3)4·5H2The mol ratio of O=1:1, takes Bi (NO3)3·5H2O and Zr (NO3)4·5H2O；
2) Bi (NO is dissolved with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O, then will dissolve the two kinds of solution mixing obtained respectively, prepare Bi3+Concentration is the precursor liquid A of 0.025～0.05mol/L；
3) regulate the pH value of precursor liquid A to 4.0～10.0, stir, be precipitated liquid B, sucking filtration, prepare white precipitate C；
4) white precipitate C is dried, prepare block, block is fully ground, obtains powder body D；
5) by the mass ratio of 1:1, the double salt that powder body D is constituted with potassium nitrate and sodium nitrate is mixed, then heat treatment 2～10h at 350～600 DEG C, prepare nanometer Bi2Zr2O7Powder body。
Step 2) it is that precursor liquid A is placed on magnetic stirring apparatus, regulate pH value with strong aqua ammonia, and adjustment process constantly produces white precipitate。
Step 2) time of stirring is 2～4h。
Step 4) described dry be that white precipitate C is placed in thermostatic drying chamber, at 60～100 DEG C, dry 5～12h。
Step 4) described in be fully ground, be that block is placed in agate mortar, be fully ground 5～20min。
Step 5) potassium nitrate and sodium nitrate constituted double salt with mass ratio for 1:1 mixing。
Step 5) it is, after the double salt agate mortar of powder body D with potassium nitrate and sodium nitrate is mixed, be placed in Muffle furnace and carry out heat treatment。
Compared with prior art, the present invention has following useful technique effect:
The present invention adopts precipitation calcination method auxiliary molten-salt growth method to prepare Bi2Zr2O7Nano material, first, adopts the sedimentation method to pass through to add corresponding precipitant, can make the slowly uniform precipitation from solution of two kinds of precipitations, calcine then through the later stage, it is thus achieved that the target product of size uniform。Secondly, there is again in conjunction with molten-salt growth method following three points advantage: (1) can reduce synthesis temperature significantly and shorten the response time, this can be attributed to the formation of the melt due to salt, makes reacted constituent mobility in the liquid phase strengthen, and diffusion rate significantly improves。Simultaneously because fused salt is applied between the granule of generation, what stop between granule is interconnected, therefore, the material soilless sticking that molten-salt growth method prepares, or only weakly agglomerated。(2) shape and size of granule can more easily be controlled；(3), in the course of reaction of molten-salt growth method and cleaning process subsequently, it is also beneficial to the elimination of impurity, forms high-purity product。The method not only technique is simple, easy to operate, and manufacturing cycle is short, and synthesis temperature is low, and cost is low, therefore has vast potential for future development。The Bi of size uniform can be prepared through the inventive method2Zr2O7Nano material, and particle diameter is little, better crystallinity degree。
Accompanying drawing explanation
Fig. 1 is the Bi that the present invention prepares when embodiment 22Zr2O7X-ray diffraction (XRD) collection of illustrative plates；
Fig. 2 is the Bi that the present invention is prepared under embodiment 2 condition2Zr2O7Scanning electron microscope (SEM) photo of nano material；Wherein, (a) is Bi under 50,000 enlargement ratios2Zr2O7The SEM figure of nano material；B () is Bi under 200,000 enlargement ratios2Zr2O7The SEM figure of nano material。
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited。
Embodiment 1
A kind of employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, comprises the following steps:
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi (NO respectively3)3·5H2O and Zr (NO3)4·5H2O, in beaker, dissolves Bi (NO with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O。After the stirring regular hour, both are mixed respectively, Bi3+Concentration is the precursor liquid A of 0.025mol/L。
2) gained precursor liquid A is placed on magnetic stirring apparatus, is slowly added dropwise strong aqua ammonia and regulates its pH=10.00, constantly have white precipitate to produce in adjustment process, stir 2h so that it is be sufficiently mixed uniformly, it is thus achieved that precipitated liquid B。
3) precipitation and magazins' layout in precipitated liquid B are washed out by the means utilizing sucking filtration, it is thus achieved that white precipitate C。
4) the white precipitate C of gained is placed in thermostatic drying chamber, controls temperature at 60 DEG C, dry 12h。The block obtained after drying is placed in agate mortar and is fully ground 10min, it is thus achieved that powder body D。
5) the powder body D obtained is mixed with potassium nitrate and sodium nitrate double salt (potassium nitrate and sodium nitrate mix with mass ratio 1:1), with the ratio of mass ratio 1:1 mix homogeneously in agate mortar, it is placed in Muffle furnace, heat treatment 6h at 550 DEG C of temperature, finally can obtain the Bi of nano-scale2Zr2O7Powder body。
Embodiment 2
A kind of employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, comprises the following steps:
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi (NO respectively3)3·5H2O and Zr (NO3)4·5H2O, in beaker, dissolves Bi (NO with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O。After the stirring regular hour, both are mixed respectively, Bi3+Concentration is the precursor liquid A of 0.03mol/L。
2) gained precursor liquid A is placed on magnetic stirring apparatus, is slowly added dropwise strong aqua ammonia and regulates its pH=10.00, constantly have white precipitate to produce in adjustment process, stir 2h so that it is be sufficiently mixed uniformly, it is thus achieved that precipitated liquid B。
3) precipitation and magazins' layout in precipitated liquid B are washed out by the means utilizing sucking filtration, it is thus achieved that white precipitate C。
4) the white precipitate C of gained is placed in thermostatic drying chamber, controls temperature at 70 DEG C, dry 10h。The block obtained after drying is placed in agate mortar and is fully ground 15min, it is thus achieved that powder body D。
5) the powder body D obtained is mixed with potassium nitrate and sodium nitrate double salt (potassium nitrate and sodium nitrate mix with mass ratio 1:1), with the ratio of mass ratio 1:1 mix homogeneously in agate mortar, it is placed in Muffle furnace, heat treatment 6h at 450 DEG C of temperature, finally can obtain the Bi of nano-scale2Zr2O7Powder body。
The Bi that the present embodiment prepares2Zr2O7X-ray diffraction (XRD) collection of illustrative plates of nano material is referring to Fig. 1, it can be seen that the present invention can prepare the Bi of pure phase under cryogenic2Zr2O7。
Referring to Fig. 2, wherein, (a) is Bi under 50,000 enlargement ratios2Zr2O7The SEM figure of nano material；B () is Bi under 200,000 enlargement ratios2Zr2O7The SEM figure of nano material。Figure it is seen that adopt precipitation calcination method auxiliary molten-salt growth method to prepare Bi2Zr2O7Particle size is between 10～20nm。
Embodiment 3
A kind of employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, comprises the following steps:
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi (NO respectively3)3·5H2O and Zr (NO3)4·5H2O, in beaker, dissolves Bi (NO with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O。After the stirring regular hour, both are mixed respectively, Bi3+Concentration is the precursor liquid A of 0.05mol/L。
2) gained precursor liquid A is placed on magnetic stirring apparatus, is slowly added dropwise strong aqua ammonia and regulates its pH=7.00, constantly have white precipitate to produce in adjustment process, stir 3h so that it is be sufficiently mixed uniformly, it is thus achieved that precipitated liquid B。
3) precipitation and magazins' layout in precipitated liquid B are washed out by the means utilizing sucking filtration, it is thus achieved that white precipitate C。
4) the white precipitate C of gained is placed in thermostatic drying chamber, controls temperature at 80 DEG C, dry 8h。The block obtained after drying is placed in agate mortar and is fully ground 5min, it is thus achieved that powder body D。
5) the powder body D obtained is mixed with potassium nitrate and sodium nitrate double salt (potassium nitrate and sodium nitrate mix with mass ratio 1:1), with the ratio of mass ratio 1:1 mix homogeneously in agate mortar, it is placed in Muffle furnace, heat treatment 10h at 350 DEG C of temperature, finally can obtain the Bi of nano-scale2Zr2O7Powder body。
Embodiment 4
A kind of employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, comprises the following steps:
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi (NO respectively3)3·5H2O and Zr (NO3)4·5H2O, in beaker, dissolves Bi (NO with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O。After the stirring regular hour, both are mixed respectively, Bi3+Concentration is the precursor liquid A of 0.04mol/L。
2) gained precursor liquid A is placed on magnetic stirring apparatus, is slowly added dropwise strong aqua ammonia and regulates its pH=7.00, constantly have white precipitate to produce in adjustment process, stir 3h so that it is be sufficiently mixed uniformly, it is thus achieved that precipitated liquid B。
3) precipitation and magazins' layout in precipitated liquid B are washed out by the means utilizing sucking filtration, it is thus achieved that white precipitate C。
4) the white precipitate C of gained is placed in thermostatic drying chamber, controls temperature at 90 DEG C, dry 7h。The block obtained after drying is placed in agate mortar and is fully ground 20min, it is thus achieved that powder body D。
5) the powder body D obtained is mixed with potassium nitrate and sodium nitrate double salt (potassium nitrate and sodium nitrate mix with mass ratio 1:1), with the ratio of mass ratio 1:1 mix homogeneously in agate mortar, it is placed in Muffle furnace, heat treatment 2h at 600 DEG C of temperature, finally can obtain the Bi of nano-scale2Zr2O7Powder body。
Embodiment 5
A kind of employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, comprises the following steps:
1) example Bi (NO in molar ratio3)3·5H2O:Zr(NO3)4·5H2O=1:1 weighs analytically pure Bi (NO respectively3)3·5H2O and Zr (NO3)4·5H2O, in beaker, dissolves Bi (NO with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O。After the stirring regular hour, both are mixed respectively, Bi3+Concentration is the precursor liquid A of 0.025mol/L。
2) gained precursor liquid A is placed on magnetic stirring apparatus, is slowly added dropwise strong aqua ammonia and regulates its pH=4.00, constantly have white precipitate to produce in adjustment process, stir 4h so that it is be sufficiently mixed uniformly, it is thus achieved that precipitated liquid B。
3) precipitation and magazins' layout in precipitated liquid B are washed out by the means utilizing sucking filtration, it is thus achieved that white precipitate C。
4) the white precipitate C of gained is placed in thermostatic drying chamber, controls temperature at 100 DEG C, dry 5h。The block obtained after drying is placed in agate mortar and is fully ground 15min, it is thus achieved that powder body D。
5) the powder body D obtained is mixed with potassium nitrate and sodium nitrate double salt (potassium nitrate and sodium nitrate mix with mass ratio 1:1), with the ratio of mass ratio 1:1 mix homogeneously in agate mortar, it is placed in Muffle furnace, heat treatment 6h at 400 DEG C of temperature, finally can obtain the Bi of nano-scale2Zr2O7Powder body。
In sum, the invention provides and a kind of synthesize simple, the cycle is short, synthesis temperature is low synthetic method-precipitation calcination method and assist molten-salt growth method to prepare Bi2Zr2O7Nano material。Precipitation calcination method auxiliary molten-salt growth method prepares the Bi of nano-scale2Zr2O7The advantage of powder body is in that: first, adopts the sedimentation method to pass through to add corresponding precipitant, can make the slowly uniform precipitation from solution of two kinds of precipitations, calcine then through the later stage, it is thus achieved that the target product of size uniform；Secondly, there is again following three points advantage in conjunction with molten-salt growth method: (1) can reduce synthesis temperature significantly and shorten the response time。This can be attributed to the formation of the melt due to salt, makes reacted constituent mobility in the liquid phase strengthen, and diffusion rate significantly improves。Simultaneously because fused salt is applied between the granule of generation, what stop between granule is interconnected, therefore, the material soilless sticking that molten-salt growth method prepares, or only weakly agglomerated。(2) shape and size of granule can more easily be controlled。(3), in the course of reaction of molten-salt growth method and cleaning process subsequently, it is also beneficial to the elimination of impurity, forms high-purity product。
Claims (7)
1. one kind adopts precipitation calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, it is characterised in that comprise the following steps:
1) by Bi (NO3)3·5H2O:Zr (NO3)4·5H2The mol ratio of O=1:1, takes Bi (NO3)3·5H2O and Zr (NO3)4·5H2O；
2) Bi (NO is dissolved with concentrated nitric acid3)3·5H2O, with deionized water dissolving Zr (NO3)4·5H2O, then will dissolve the two kinds of solution mixing obtained respectively, prepare Bi3+Concentration is the precursor liquid A of 0.025～0.05mol/L；
3) regulate the pH value of precursor liquid A to 4.0～10.0, stir, be precipitated liquid B, sucking filtration, prepare white precipitate C；
4) white precipitate C is dried, prepare block, block is fully ground, obtains powder body D；
5) by the mass ratio of 1:1, the double salt that powder body D is constituted with potassium nitrate and sodium nitrate is mixed, then heat treatment 2～10h at 350～600 DEG C, prepare nanometer Bi2Zr2O7Powder body。
2. according to claim 1 employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, it is characterised in that step 2) it is that precursor liquid A is placed on magnetic stirring apparatus, regulate pH value with strong aqua ammonia, and adjustment process constantly produces white precipitate。
3. according to claim 1 employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, it is characterised in that step 2) time of stirring is 2～4h。
4. according to claim 1 employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, it is characterised in that step 4) described dry be that white precipitate C is placed in thermostatic drying chamber, at 60～100 DEG C, dry 5～12h。
5. according to claim 1 employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, it is characterised in that step 4) described in be fully ground, be that block is placed in agate mortar, be fully ground 5～20min。
6. according to claim 1 employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, it is characterised in that step 5) potassium nitrate and sodium nitrate constituted double salt with mass ratio for 1:1 mixing。
7. according to claim 1 employing precipitates calcination method auxiliary molten-salt growth method preparation nanometer Bi2Zr2O7The method of powder body, it is characterised in that step 5) it is, after the double salt agate mortar of powder body D with potassium nitrate and sodium nitrate is mixed, be placed in Muffle furnace and carry out heat treatment。
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Cited By (3)
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| CN106564948A (en) * | 2016-10-18 | 2017-04-19 | 陕西科技大学 | Method for preparing granular Bi2Zr2O7 nano material through non-hydrolytic sol-gel auxiliary molten-salt growth method |
| CN106629844A (en) * | 2016-10-18 | 2017-05-10 | 陕西科技大学 | Method for preparing bulk Bi2Zr2O7 nanocrystalline by template method assisted sintering method |
| CN112125281A (en) * | 2020-10-28 | 2020-12-25 | 中国科学院上海应用物理研究所 | Method for preparing lanthanide oxide material by using coprecipitation combined with molten salt deposition method and application thereof |
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| CN104843787A (en) * | 2015-04-23 | 2015-08-19 | 中国地质大学（武汉） | Preparation method of cubic lanthanum zirconate nanometer monocrystal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106564948A (en) * | 2016-10-18 | 2017-04-19 | 陕西科技大学 | Method for preparing granular Bi2Zr2O7 nano material through non-hydrolytic sol-gel auxiliary molten-salt growth method |
| CN106629844A (en) * | 2016-10-18 | 2017-05-10 | 陕西科技大学 | Method for preparing bulk Bi2Zr2O7 nanocrystalline by template method assisted sintering method |
| CN106564948B (en) * | 2016-10-18 | 2017-12-05 | 陕西科技大学 | A kind of non-hydrolytic sol-gel auxiliary molten-salt growth method prepares graininess Bi2Zr2O7The method of nano material |
| CN106629844B (en) * | 2016-10-18 | 2018-08-17 | 陕西科技大学 | A kind of template assisted sintering method preparation bulk Bi2Zr2O7Nanocrystalline method |
| CN112125281A (en) * | 2020-10-28 | 2020-12-25 | 中国科学院上海应用物理研究所 | Method for preparing lanthanide oxide material by using coprecipitation combined with molten salt deposition method and application thereof |
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Application publication date: 20160622 |