CN105800685A - Preparation method of regular octahedral bismuth fluoride material - Google Patents
Preparation method of regular octahedral bismuth fluoride material Download PDFInfo
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Abstract
The invention relates to a preparation method of a regular octahedral bismuth fluoride material. The method comprises the following steps: (1) dissolving bismuth fluoride into deionized water, adding concentrated nitric acid and preparing a bismuth nitrate solution with the molar concentration of 45-55mM; (2) dissolving sodium fluoride into the deionized water and adding polyvinylpyrrolidone to prepare a sodium fluoride solution with the molar concentration of 37.5-125mM; (3) adding the bismuth nitrate solution to the sodium fluoride solution, carrying out standing reaction at 20-30 DEG C to obtain a sediment, wherein the volume ratio of the bismuth nitrate solution to the sodium fluoride solution is 1 to (3.5-4.5); and (4) filtering, washing and drying the sediment obtained in the step (3) to obtain the regular octahedral bismuth fluoride material. According to the preparation method, the regular octahedral bismuth fluoride material can be synthesized by one-step reaction; the cost is saved; the environment is protected; and the product is high in purity, uniform and regular in shape and size, and beneficial to large-scale mass production in future.
Description
Technical field
The preparation method that the present invention relates to fluoride bismuth, the preparation method being specifically related to a kind of regular octahedron shape fluoride bismuth material.
Background technology
In recent years, Bi based compound is noticeable because having special layer structure and appropriately sized energy gap.As a kind of metal fluoride positive electrode, BiF3Reacted by reversible transformation, it is thus achieved that high storage volume.Although BiF3Specific energy be only 905Wh/kg, but its energy density per unit volume is up to 7170Wh/l.BiF3As the typical ionic compound of one, the positive electrode of secondary cell can be made with the elements doped lithium such as carbon and silver, and all quantivalences of material can be made full use of, advantages such as so making to have in electrode process exchange electronics is many, cell voltage is high and energy density is big, along with the research that it is more deep, BiF3Promising a new generation lithium ion secondary battery anode material will be become.
At present, preparation BiF3Method usually oxide/sulfide/the hydroxide etc. of bismuth (III) is carried out in HF atmosphere gas-solid phase reaction, or at a certain temperature, F2Gas passes through bismuth metal powder, and gas-solid phase reaction occurs.This kind of reaction time consumption, power consumption and environmental pollution are big, thus valuable product.Additionally, precipitate out Bismuth hydrate. in alkaline solution by bismuth (III) ion in mannitol chelating five water bismuth nitrate, Bismuth hydrate. stirs 12h in HF solution and occurs solid-liquid reaction to generate BiF3Theoretical method on feasible, but actual yield is very low, and impurity is many and product is unstable.
The preparation method that Chinese invention patent (CN101212050A) discloses a kind of bismuth trifluoride anode material of Li secondary battery, specifically includes and bismuth salt is dissolved in acetum preparation bismuth salt acetum, add surfactant；Preparation solubility villiaumite or HF ethanol water, obtain alcohol fluorine mixed solution simultaneously；At 0～45 DEG C, mix two kinds of solution obtain BiF3Precipitate, then filtration washing is dried, and obtains BiF3Product, but this preparation method can not obtain specific morphology fluoride bismuth.Therefore current, not yet it is related at room temperature prepare the report of the synthetic technology of regular octahedron fluoride bismuth material.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of can the preparation method of at room temperature one-step synthesis regular octahedron shape fluoride bismuth material.
Technical scheme provided by the present invention is:
The preparation method of a kind of regular octahedron shape fluoride bismuth material, comprises the steps:
1) bismuth nitrate being dissolved in deionized water, add concentrated nitric acid, preparation molar concentration is the bismuth nitrate solution of 45～55mM；
2) sodium fluoride being dissolved in deionized water, add polyvinylpyrrolidone, preparation molar concentration is the Fluorinse of 37.5～125mM；
3) bismuth nitrate solution is joined in Fluorinse, standing and reacting at 20～30 DEG C, it is precipitated thing；The volume ratio of described bismuth nitrate solution and Fluorinse is: 1:3.5～4.5；
4) by step 3) in the precipitate that obtains filter, washing, dry, namely obtain regular octahedron shape fluoride bismuth material.
In technique scheme, water solution system under room temperature is adopted to react, using bismuth nitrate as bismuth source, sodium fluoride is as fluorine source, it is simultaneously introduced concentrated nitric acid and polyvinylpyrrolidone, by controlling raw material type, concentration, reaction temperature and the volume ratio between solution, it is possible to obtain the regular octahedron of pattern, size uniformity rule.Achieve the simplification of preparation method, it is not necessary to use any firing equipment, it is to avoid energy waste；Do not use the surfactant that strong toxicity, price are high, save cost and protect environment；Wherein bismuth nitrate is common bismuth salt, and sodium fluoride is common villiaumite, and both of which is less costly, prepares gained regular octahedron shape fluoride bismuth material purity high, is conducive to large-scale mass production from now on.
As preferably, described step 1) in the volume ratio of bismuth nitrate solution and concentrated nitric acid be 20:1.2～0.8.Add concentrated nitric acid and be conducive to the dissolving in deionized water of bismuth nitrate crystal, neutralize that sodium fluoride is soluble in water and the alkalescence that produces so that solution is in neutral state, is conducive to octahedral formation simultaneously.
As preferably, described step 2) in the mass concentration of polyvinylpyrrolidone be 6.2～37.5g/L.The polyvinylpyrrolidone added is a kind of good dispersant, can effectively control being uniformly distributed of nucleus, it is to avoid reunite so that octahedron can grow equably.
As preferably, described step 1) in the concentration of bismuth nitrate solution of preparation be 48～53mM.
As preferably, described step 2) in the concentration of Fluorinse of preparation be 60～125mM.
As preferably, described step 4) in precipitate respectively wash 3～5 times by deionized water and dehydrated alcohol.
As preferably, described step 1) in the concentration of bismuth nitrate solution of preparation be 48～52mM, the volume ratio of bismuth nitrate solution and concentrated nitric acid is 20:1.1～0.9；Described step 2) in the concentration of Fluorinse of preparation be 100～125mM, the mass concentration of polyvinylpyrrolidone is 20～30g/L；The volume ratio of described bismuth nitrate solution and Fluorinse is: 1:3.8～4.2.In technique scheme, the technological parameters such as the mass concentration of the volume ratio of the concentration of the bismuth nitrate solution adopted, bismuth nitrate solution and concentrated nitric acid, the concentration of Fluorinse and polyvinylpyrrolidone are mutually worked in coordination with, are influenced each other, making the pattern of product regular octahedron shape fluoride bismuth material of gained, the more homogeneous rule of size, purity is higher.
As it is preferred that, described step 3) in stir standing and reacting 4～6 days.
Compared with the existing technology, beneficial effects of the present invention is embodied in:
(1) preparation method provided by the present invention has only to single step reaction at ambient temperature and just can synthesize regular octahedron shape fluoride bismuth material；
(2) preparation method provided by the present invention need not use any firing equipment, it is to avoid energy waste；Do not use the surfactant that strong toxicity, price are high, save cost and protect environment；
(3) gained regular octahedron shape fluoride bismuth material not only purity is prepared high, and the homogeneous rule of appearance and size, be conducive to large-scale mass production from now on.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the regular octahedron shape fluoride bismuth material that embodiment 1 prepares；
Fig. 2 is the scanning electron microscope (SEM) photograph of 12000 times of the regular octahedron shape fluoride bismuth material that embodiment 1 prepares；
Fig. 3 is the scanning electron microscope (SEM) photograph of 50000 times of the regular octahedron shape fluoride bismuth material that embodiment 1 prepares；
Fig. 4 is the transmission electron microscope picture of the regular octahedron shape fluoride bismuth material that embodiment 1 prepares；
Fig. 5 is the scanning electron microscope (SEM) photograph of 12000 times of the regular octahedron shape fluoride bismuth material that embodiment 2 prepares；
Fig. 6 is the scanning electron microscope (SEM) photograph of 24000 times of the regular octahedron shape fluoride bismuth material that embodiment 3 prepares；
Fig. 7 is the scanning electron microscope (SEM) photograph of 24000 times of the regular octahedron shape fluoride bismuth material that embodiment 4 prepares；
Fig. 8 is the scanning electron microscope (SEM) photograph of 24000 times of the material that comparative example 1 prepares；
Fig. 9 is the scanning electron microscope (SEM) photograph of 8000 times of the material that comparative example 2 prepares；
Figure 10 is the scanning electron microscope (SEM) photograph of 6000 times of the material that comparative example 3 prepares；
Figure 11 is the scanning electron microscope (SEM) photograph of 15000 times of the material that comparative example 4 prepares；
Figure 12 is the scanning electron microscope (SEM) photograph of 20000 times of the material that comparative example 5 prepares.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described:
The present invention adopts Normal Temperature Hydrolysis to synthesize, and agents useful for same is analytical pure.
Adopting Rigaku D/max-rB rotating anode x-ray diffractometer to analyze the crystal phase structure of sample, X ray is Cu target K α (λ=0.15406nm), voltage 45kV, electric current 40mA；Slit DS:1 °, SS:1 °, RS:1 °；Step-length: 0.02 °；Sweep limits 10 °-90 °；5 °/min of sweep speed.The pattern of sample is by FEI-QuantaFEG650 type sem observation.
Embodiment 1
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 1mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mM；0.42gNaF is dissolved in the deionized water of 80ml, adds 2gPVP, be configured to the Fluorinse that concentration is 0.125M；Bismuth nitrate solution is added in Fluorinse, standing and reacting 5 days after stirring；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven, namely obtain regular octahedron shape fluoride bismuth material.
Regular octahedron shape fluoride bismuth material is carried out X-ray diffraction analysis, and result, as it is shown in figure 1, the fluoride bismuth composition of preparation is single, belongs to centroid cubic crystal system (JCPDS51-0944), Fm3m space group, and has significantly high degree of crystallinity.
Regular octahedron shape fluoride bismuth material is scanned electronic microscope photos, and as shown in Figures 2 and 3, the sample of embodiment 1 preparation is made up of the micro nano structure of regular octahedron, and regular octahedron structural style is single, uniform, regular.From high power stereoscan photograph it can be seen that every piece of octahedral length of side is about～2 μm.From the transmission electron microscope photo of Fig. 4 sample it can be seen that the sample of embodiment 1 preparation is solid construction.
Embodiment 2
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 1mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mmol/L；0.42gNaF is dissolved in the deionized water of 80ml, adds 0.5gPVP, be configured to the NaF solution that concentration is 0.125mol/L；Bismuth nitrate solution is added in Fluorinse, after stirring at 25 DEG C standing and reacting 5 days；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven, namely obtain regular octahedron shape fluoride bismuth material.Products obtained therefrom is scanned electronic microscope photos, as it is shown in figure 5, be made up of the micro nano structure of regular octahedron, regular octahedron structural style is single, uniform, regular.
Embodiment 3
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 1mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mmol/L；0.42gNaF is dissolved in the deionized water of 80ml, adds 3gPVP, be configured to the NaF solution that concentration is 0.125mol/L；Bismuth nitrate solution is added in Fluorinse, after stirring at 25 DEG C standing and reacting 5 days；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven, namely obtain regular octahedron shape fluoride bismuth material.Products obtained therefrom being scanned electronic microscope photos, as shown in Figure 6, is made up of the micro nano structure of regular octahedron, regular octahedron structural style is single, uniform, regular.
Embodiment 4
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 1mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mmol/L；0.126gNaF is dissolved in the deionized water of 80ml, adds 2gPVP, be configured to the NaF solution that concentration is 0.0375mol/L；Bismuth nitrate solution is added in Fluorinse, after stirring at 25 DEG C standing and reacting 5 days；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven, namely obtain regular octahedron shape fluoride bismuth material.Products obtained therefrom is scanned electronic microscope photos, as it is shown in fig. 7, be made up of the micro nano structure of regular octahedron, regular octahedron structural style is single, uniform, regular.
Comparative example 1
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 1mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mmol/L；0.084gNaF is dissolved in the deionized water of 80ml, adds 2gPVP, be configured to the NaF solution that concentration is 0.025mol/L；Bismuth nitrate solution is added in Fluorinse, after stirring at 25 DEG C standing and reacting 5 days；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven.Products obtained therefrom is scanned electronic microscope photos, as shown in Figure 8, the micro nano structure composition of pattern essentially regular octahedron, but there is cotton-shaped or membranaceous impurity in surface, regular octahedron corner angle fuzzy, the no longer homogeneous rule of pattern, the concentration mainly due to Fluorinse reduces, and bismuth nitrate solution is excessive.
Comparative example 2
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 1mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mmol/L；0.84gNaF is dissolved in the deionized water of 80ml, adds 2gPVP, be configured to the NaF solution that concentration is 0.25mol/L；Bismuth nitrate solution is added in Fluorinse, after stirring at 25 DEG C standing and reacting 5 days；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven.Products obtained therefrom is scanned electronic microscope photos, as it is shown in figure 9, the pattern of gained is no longer regular octahedron, main reason is that the concentration of Fluorinse is excessive, affect the growth of regular octahedron pattern.
Comparative example 3
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 1mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mmol/L；By 0.37gNH4F is dissolved in the deionized water of 80ml, adds 2gPVP, is configured to the NH that concentration is 0.125mol/L4F solution；Bismuth nitrate solution is added in ammonium fluoride solution, after stirring at 25 DEG C standing and reacting 5 days；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven.Products obtained therefrom is scanned electronic microscope photos, and as shown in Figure 10, the pattern of gained is no longer regular octahedron, main reason is that ammonium fluoride is selected in fluorine source, and ammonium salt can affect octahedral formation with acidity.
Comparative example 4
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 1mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mmol/L；0.42gNaF is dissolved in the deionized water of 80ml, adds 2gPVP, be configured to the NaF solution that concentration is 0.125mol/L；Bismuth nitrate solution is added in Fluorinse, after stirring at 35 DEG C standing and reacting 5 days；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven.Products obtained therefrom is scanned electronic microscope photos, as shown in figure 11, the micro nano structure composition of pattern essentially regular octahedron, but there is depression, breach in regular octahedron surface, main reason is that standing and reacting temperature is too high, have influence on nucleation and the slowly growth of regular octahedron pattern.
Comparative example 5
By 0.485gBi (NO3)3·5H2O is dissolved in the deionized water of 19ml, adds 0.6mlHNO3, it is configured to the bismuth nitrate solution that concentration is 50mmol/L；0.42gNaF is dissolved in the deionized water of 80ml, adds 2gPVP, be configured to the NaF solution that concentration is 0.125mol/L；Bismuth nitrate solution is added in Fluorinse, after stirring at 25 DEG C standing and reacting 5 days；The precipitate obtained respectively is cleaned 3 times with deionized water and dehydrated alcohol respectively, 60 DEG C of dry 12h in air dry oven.Products obtained therefrom is scanned electronic microscope photos, and as shown in figure 12, the pattern of gained is spherical, the HNO that main cause adds3Very few so that solution alkaline, affect octahedral growth.
Claims (8)
1. the preparation method of a regular octahedron shape fluoride bismuth material, it is characterised in that comprise the steps:
1) bismuth nitrate being dissolved in deionized water, add concentrated nitric acid, preparation molar concentration is the bismuth nitrate solution of 45～55mM；
2) sodium fluoride being dissolved in deionized water, add polyvinylpyrrolidone, preparation molar concentration is the Fluorinse of 37.5～125mM；
3) bismuth nitrate solution is joined in Fluorinse, standing and reacting at 20～30 DEG C, it is precipitated thing；The volume ratio of described bismuth nitrate solution and Fluorinse is: 1:3.5～4.5；
4) by step 3) in the precipitate that obtains filter, washing, dry, namely obtain regular octahedron shape fluoride bismuth material.
2. the preparation method of regular octahedron shape fluoride bismuth material according to claim 1, it is characterised in that described step 1) in the volume ratio of bismuth nitrate solution and concentrated nitric acid be 20:1.2～0.8.
3. the preparation method of regular octahedron shape fluoride bismuth material according to claim 2, it is characterised in that described step 2) in the mass concentration of polyvinylpyrrolidone be 6.2～37.5g/L.
4. the preparation method of regular octahedron shape fluoride bismuth material according to claim 1, it is characterised in that described step 1) in the concentration of bismuth nitrate solution of preparation be 48～53mM.
5. the preparation method of regular octahedron shape fluoride bismuth material according to claim 1, it is characterised in that described step 2) in the concentration of Fluorinse of preparation be 60～125mM.
6. the preparation method of regular octahedron shape fluoride bismuth material according to claim 1, it is characterised in that described step 4) in precipitate respectively wash 3～5 times by deionized water and dehydrated alcohol.
7. the preparation method of regular octahedron shape fluoride bismuth material according to claim 3, it is characterised in that described step 1) in the concentration of bismuth nitrate solution of preparation be 48～52mM, the volume ratio of bismuth nitrate solution and concentrated nitric acid is 20:1.1～0.9；Described step 2) in the concentration of Fluorinse of preparation be 100～125mM, the mass concentration of polyvinylpyrrolidone is 20～30g/L；The volume ratio of described bismuth nitrate solution and Fluorinse is: 1:3.8～4.2.
8. the preparation method of the regular octahedron shape fluoride bismuth material according to claim 1 or 7, it is characterised in that described step 3) in stir standing and reacting 4～6 days.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111186856A (en) * | 2018-11-14 | 2020-05-22 | 多氟多化工股份有限公司 | Preparation method of bismuth trifluoride |
| CN111218697A (en) * | 2020-01-09 | 2020-06-02 | 浙江工业大学 | Pb electrode with octahedral crystal face, preparation method and application thereof |
| CN115259219A (en) * | 2022-07-22 | 2022-11-01 | 承德莹科精细化工股份有限公司 | Preparation method of photoelectric material additive bismuth trifluoride |
-
2016
- 2016-03-09 CN CN201610133279.XA patent/CN105800685B/en active Active
Non-Patent Citations (1)
| Title |
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| ALBERTO ESCUDERO ET. AL: "Synthesis and luminescence of uniform europiumdoped bismuth fluoride and bismuth oxyfluoride particles with different morphologies", 《CRYSTENGCOMM》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111186856A (en) * | 2018-11-14 | 2020-05-22 | 多氟多化工股份有限公司 | Preparation method of bismuth trifluoride |
| CN111186856B (en) * | 2018-11-14 | 2022-12-02 | 多氟多新材料股份有限公司 | Preparation method of bismuth trifluoride |
| CN111218697A (en) * | 2020-01-09 | 2020-06-02 | 浙江工业大学 | Pb electrode with octahedral crystal face, preparation method and application thereof |
| CN111218697B (en) * | 2020-01-09 | 2021-02-19 | 浙江工业大学 | Pb electrode with octahedral crystal face, preparation method and application thereof |
| CN115259219A (en) * | 2022-07-22 | 2022-11-01 | 承德莹科精细化工股份有限公司 | Preparation method of photoelectric material additive bismuth trifluoride |
| CN115259219B (en) * | 2022-07-22 | 2024-02-20 | 承德莹科精细化工股份有限公司 | Preparation method of photoelectric material additive bismuth trifluoride |
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