CN105481017A - Preparation method of sodium bismuth molybdate-tungstate nano material - Google Patents
Preparation method of sodium bismuth molybdate-tungstate nano material Download PDFInfo
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- CN105481017A CN105481017A CN201610044992.7A CN201610044992A CN105481017A CN 105481017 A CN105481017 A CN 105481017A CN 201610044992 A CN201610044992 A CN 201610044992A CN 105481017 A CN105481017 A CN 105481017A
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- bismuth
- sodium
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- glycerine
- tungstate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/006—Compounds containing, besides tungsten, two or more other elements, with the exception of oxygen or hydrogen
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- 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
The invention relates to a preparation method of a sodium bismuth molybdate-tungstate nano material, and belongs to the technical field of novel nano materials. The preparation method comprises the following steps: S1, in an isopropanol solvent, solvothermal reaction between bismuth nitrate and glycerin mixed liquid is carried out to prepare bismuth glycerolate; S2, bismuth glycerolate is uniformly dispersed in a mixed aqueous solution of sodium molybdate and sodium tungstate for hydrothermal reaction, so as to obtain nano sodium bismuth molybdate-tungstate. Compared with the prior art, the preparation method has the following major advantages: sodium bismuth molybdate-tungstate prepared by adopting the preparation method is characterized in that nanocrystalline is replaced by molybdate and tungstate lattices, the defect that the heating effect of molybdate results in laser attenuation is overcome, at the same time the preparation processing equipment is simple, and the preparation process is low in temperature and small in energy consumption; the product, namely sodium bismuth molybdate (NaBi(Mo<x>W<1-x>O<4>)<2>, wherein x=0.1-0.9) prepared by adopting the preparation method is 20-50 nm in grain size, has the advantage of low sintering temperature, can be used for preparing a rare earth doping laser host material, and can also be used as a luminescent material.
Description
Technical field
The present invention relates to a kind of preparation method of molybdenum sodium bismuth tungstate nano material, belong to nanometer new material technology field.
Background technology
With it, molybdate compound has that luminous efficiency is high, chemical stability good, anti-good fortune is penetrated and the excellent characteristic such as anti-high light lesion capability is large, at luminescent material, the aspects such as scintillation crystal all have a wide range of applications.Along with laser Application Areas is to the miniaturization of device, microplate, the requirement of high efficiency and the development of semiconductor laser, molybdic acid salt laser crystals has become a hot research object.Molybdate has large absorption, emission cross section and from features such as birefringent tunable as laser crystals, but molybdate self has the shortcomings such as heat effect, research finds to utilize the randomness of the anion doped structure caused can make this crystal-like absorption spectrum inhomogeneous broadening, thus improve thermal characteristics, this randomness also helps the high-concentration dopant of rare earth ion in addition.Therefore, utilizing tungstate ion to replace part molybdenum acid ion synthesis nitration mixture salt is one of developing direction improving molybdate crystal performance.Due to bismuth metal ion (Bi
3+) and rare earth element ion (RE
3+) radius and chemical property close, be easy to the doping realizing rare earth ion, therefore prepare luminescent material and laser host material that molybdenum sodium bismuth tungstate composite salt can obtain high stability.
At present, bismuth molybdate sodium and sodium bismuth tungstate material adopt solid phase melting method, low-temperature combustion method, sol-gel method, spray heating decomposition, freeze-drying mostly, and prepared by hydrothermal method, wherein hydrothermal method preparation temperature is low, and energy consumption is low.
Summary of the invention
The invention provides a kind of employing solvent-thermal method in conjunction with hydro-thermal legal system for molybdenum sodium bismuth tungstate (NaBi (Mo
xw
1-xo
4)
2, x=0.1-0.9) and nano material, prepared nano material has high-luminous-efficiency, can be used for High-performance lasers substrate material and kernel analysis instrument scintillator material.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation method of molybdenum sodium bismuth tungstate nano material, is characterized in that including following steps:
S1 is in isopropanol solvent, and Bismuth trinitrate and glycerine mixed solution solvent thermal reaction obtain glycerine bismuth;
Glycerine bismuth is dispersed in Sodium orthomolybdate and sodium wolframate mixed aqueous solution by S2, and hydro-thermal reaction obtains nanometer molybdenum sodium bismuth tungstate.
By such scheme, molybdenum sodium bismuth tungstate molecular formula is NaBi (Mo
xw
1-xo
4)
2, wherein, x=0.1-0.9.
By such scheme, solvent thermal reaction described in step S1 obtains in glycerine bismuth, Bismuth trinitrate molfraction is 1, glycerine molfraction 1.5-3, both are dissolved in the Virahol of molfraction 100-500 together, stir, 150-200 DEG C of solvent thermal reaction 1-24 hour in autoclave, then naturally cool to room temperature, filter to isolate glycerine bismuth ((Bi
2(OCH
2cHOHCH
2o)
3)) pressed powder, 80-100 DEG C of dry for standby.
By such scheme, hydro-thermal reaction described in step S2 obtains in nanometer molybdenum sodium bismuth tungstate, Sodium orthomolybdate (NaMoO
42H
2o) with sodium wolframate (Na
2wO
42H
2o) total molfraction is 4 parts, wherein mole accounting of Sodium orthomolybdate and sodium wolframate is at 0.1-0.9, concentration of aqueous solution counts 0.2-2 mol/L with sodium ion, then adds the glycerine bismuth that molfraction is 1 part, and strong stirring makes glycerine bismuth be uniformly dispersed, then use between nitric acid adjust ph to 0-2, react under hydrothermal condition in autoclave, then naturally cool to room temperature, filter and repeatedly use deionized water wash product, 80-150 DEG C of oven dry, the molybdenum sodium bismuth tungstate nanometer powder obtained.
By such scheme, described hydrothermal temperature 160-200 DEG C, hydro-thermal reaction time 1-24 hour,
By such scheme, the average grain size of nanometer molybdenum sodium bismuth tungstate is 20-50nm.
Reaction mechanism of the present invention.
(1) the first step solvent-thermal process glycerine bismuth title complex
(2) second step Hydrothermal Synthesis
molybdenumsodium bismuth tungstate
The present invention is relative to the major advantage of prior art: molybdenum sodium bismuth tungstate prepared by the present invention is that molybdate and tungstate lattice substitute nanocrystalline, overcome the shortcoming that molybdate heat effect causes laser attenuation, preparation technology's equipment is simple simultaneously, and preparation technology's temperature is low, and energy consumption is little.Products obtained therefrom bismuth molybdate sodium (NaBi (Mo of the present invention
xw
1-xo
4)
2, x=0.1-0.9) grain-size at 20-50nm, there is the advantage that sintering temperature is low, can be used as preparation rear-earth-doped laser host material, also can be used as luminescent material.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with embodiment, the present invention is described in further detail, but embodiment is not construed as limiting the invention.
Embodiment 1:
1) get 10mmol Bismuth trinitrate, 30mmol glycerine is dissolved in the Virahol of 5mol (about 382ml), stirs and obtains clear liquor, and this solution being transferred to volume is in the autoclave of 500ml, is warming up to 160 DEG C and is incubated 6 hours.After stopping heating, question response still is cooled to room temperature, and filter and use washed with isopropyl alcohol filter cake 3 times, filter cake, 80 DEG C of dryings 12 hours, obtains glycerine bismuth meal body;
2) 8mmol Sodium orthomolybdate (Na is got
2moO
42H
2and 8mmol sodium wolframate (Na O)
2wO
42H
2o) be dissolved in 100ml (sodium ion total concn 0.32mol/L) deionized water, then join in above-mentioned deionized water solution by 4mmol glycerine bismuth, strong stirring is that glycerine bismuth is uniformly dispersed, between nitric acid adjust ph to 0-1.Mixed solution being transferred to volume is in the autoclave of 150ml again, heats up 180 DEG C and be incubated 12 hours.After stopping heating, question response still is cooled to room temperature, and filter and use deionized water wash 3 times, filter cake, 120 DEG C of dryings 12 hours, obtains target product molybdenum sodium bismuth tungstate (NaBi (Mo
0.5w
0.5o
4)
2) nano-powder, nanocrystal median size 30nm.
Embodiment 2:
1) get 10mol Bismuth trinitrate, 15mol glycerine is dissolved in the Virahol of 1000mol (76.4L), stirs and obtains clear liquor, and this solution being transferred to volume is in the autoclave of 100l, is warming up to 160 DEG C and is incubated 12 hours.After stopping heating, question response still is cooled to room temperature, and filter and use washed with isopropyl alcohol filter cake 3 times, filter cake, 80 DEG C of dryings 12 hours, obtains glycerine bismuth meal body;
2) 6mol Sodium orthomolybdate (Na is got
2moO
42H
2and 4mol sodium wolframate (Na O)
2wO
42H
2o) be dissolved in 10l (sodium ion total concn 0.2mol/L) deionized water, again 2.5mol glycerine bismuth is joined in above-mentioned deionized water solution, strong stirring is that glycerine bismuth is uniformly dispersed, between nitric acid adjust ph to 1-2, mixed solution being transferred to volume is in the autoclave of 15L again, heats up 180 DEG C and be incubated 24 hours.After stopping heating, question response still is cooled to room temperature, and filter and use deionized water wash filter cake 3 times, filter cake, 120 DEG C of dryings 12 hours, obtains target product molybdenum sodium bismuth tungstate (NaBi (Mo
0.6w
0.4o
4)
2) nano-powder, nanocrystal median size 35nm.
Embodiment 3:
1) get 100mmol Bismuth trinitrate, 200mmol glycerine is dissolved in the Virahol of 32.7mol (2.5l), stirs and obtains clear liquor, and this solution being transferred to volume is in the autoclave of 4l, is warming up to 160 DEG C and is incubated 3 hours.After stopping heating, question response still is cooled to room temperature, and filter and use washed with isopropyl alcohol filter cake 3 times, filter cake, 80 DEG C of dryings 12 hours, obtains glycerine bismuth meal body;
2) 90mmol Sodium orthomolybdate (Na is got
2moO
42H
2and 10mol sodium wolframate (Na O)
2wO
42H
2o) be dissolved in 700ml deionized water, join in above-mentioned deionized water solution by 25mmol glycerine bismuth again, strong stirring is that glycerine bismuth is uniformly dispersed, between nitric acid adjust ph to 0-1, mixed solution being transferred to volume is in the autoclave of 1000ml again, heats up 180 DEG C and be incubated 4 hours.After stopping heating, question response still is cooled to room temperature, and filter and use deionized water wash filter cake 3 times, filter cake, 120 DEG C of dryings 12 hours, obtains target product molybdenum sodium bismuth tungstate (NaBi (Mo
0.9w
0.1o
4)
2) nano-powder, nanocrystal median size 25nm.
Embodiment 4:
1) get 100mmol Bismuth trinitrate, 200mmol glycerine is dissolved in the Virahol of 32.7mol (2.5l), stirs and obtains clear liquor, and this solution being transferred to volume is in the autoclave of 4l, is warming up to 180 DEG C and is incubated 3 hours.After stopping heating, question response still is cooled to room temperature, and filter and use washed with isopropyl alcohol filter cake 3 times, filter cake, 80 DEG C of dryings 12 hours, obtains glycerine bismuth meal body;
2) 10mmol Sodium orthomolybdate (Na is got
2moO
42H
2and 90mol sodium wolframate (Na O)
2wO
42H
2o) be dissolved in 800ml deionized water, join in above-mentioned deionized water solution by 25mmol glycerine bismuth again, strong stirring is that glycerine bismuth is uniformly dispersed, between nitric acid adjust ph to 0-1, mixed solution being transferred to volume is in the autoclave of 1000ml again, heats up 200 DEG C and be incubated 24 hours.After stopping heating, question response still is cooled to room temperature, and filter and use deionized water wash filter cake 3 times, filter cake, 120 DEG C of dryings 12 hours, obtains target product molybdenum sodium bismuth tungstate (NaBi (Mo
0.1w
0.9o
4)
2) nano-powder, nanocrystal median size 40nm.
Claims (6)
1. a preparation method for molybdenum sodium bismuth tungstate nano material, is characterized in that including following steps:
S1 is in isopropanol solvent, and Bismuth trinitrate and glycerine mixed solution solvent thermal reaction obtain glycerine bismuth;
Glycerine bismuth is dispersed in Sodium orthomolybdate and sodium wolframate mixed aqueous solution by S2, and hydro-thermal reaction obtains nanometer molybdenum sodium bismuth tungstate.
2. the preparation method of molybdenum sodium bismuth tungstate nano material according to claim 1, is characterized in that molybdenum sodium bismuth tungstate molecular formula is NaBi (Mo
xw
1-xo
4)
2, wherein, x=0.1-0.9.
3. the preparation method of molybdenum sodium bismuth tungstate nano material according to claim 1, it is characterized in that, solvent thermal reaction described in step S1 obtains in glycerine bismuth, and Bismuth trinitrate molfraction is 1, glycerine molfraction 1.5-3, both are dissolved in the Virahol of molfraction 100-500 together, stir, in autoclave, 150-200 DEG C of solvent thermal reaction 1-24 hour, then naturally cools to room temperature, filter to isolate glycerine bismuth pressed powder, 80-100 DEG C of dry for standby.
4. the preparation method of molybdenum sodium bismuth tungstate nano material according to claim 1, it is characterized in that, hydro-thermal reaction described in step S2 obtains in nanometer molybdenum sodium bismuth tungstate, Sodium orthomolybdate and the total molfraction of sodium wolframate are 4 parts, wherein mole accounting of Sodium orthomolybdate and sodium wolframate is at 0.1-0.9, concentration of aqueous solution counts 0.2-2 mol/L with sodium ion, add the glycerine bismuth that molfraction is 1 part again, strong stirring makes glycerine bismuth be uniformly dispersed, then use between nitric acid adjust ph to 0-2, react under hydrothermal condition in autoclave, then room temperature is naturally cooled to, filter and repeatedly use deionized water wash product, 80-150 DEG C of oven dry, the molybdenum sodium bismuth tungstate nanometer powder obtained.
5. the preparation method of molybdenum sodium bismuth tungstate nano material according to claim 4, is characterized in that, described hydrothermal temperature 160-200 DEG C, hydro-thermal reaction time 1-24 hour.
6. the preparation method of molybdenum sodium bismuth tungstate nano material according to claim 1, is characterized in that, the average grain size of nanometer molybdenum sodium bismuth tungstate is 20-50nm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105879855A (en) * | 2016-04-27 | 2016-08-24 | 武汉工程大学 | Graphene-gamma-bismuth molybdate nano-composite material, method for preparing same and application of graphene-gamma-bismuth molybdate nano-composite material |
| CN105967235A (en) * | 2016-04-27 | 2016-09-28 | 武汉工程大学 | Graphene-sodium bismuth molybdate nano composite material and preparation method and application thereof |
| CN107032401A (en) * | 2017-05-27 | 2017-08-11 | 武汉工程大学 | A kind of bismuth molybdate sodium nano material and preparation method thereof |
| CN107055614A (en) * | 2017-05-27 | 2017-08-18 | 武汉工程大学 | A kind of bismuth molybdate potassium nano material and preparation method thereof |
| CN108213453A (en) * | 2018-01-25 | 2018-06-29 | 叶剑 | A kind of preparation method of more metal nano materials |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105879855A (en) * | 2016-04-27 | 2016-08-24 | 武汉工程大学 | Graphene-gamma-bismuth molybdate nano-composite material, method for preparing same and application of graphene-gamma-bismuth molybdate nano-composite material |
| CN105967235A (en) * | 2016-04-27 | 2016-09-28 | 武汉工程大学 | Graphene-sodium bismuth molybdate nano composite material and preparation method and application thereof |
| CN105967235B (en) * | 2016-04-27 | 2017-10-10 | 武汉工程大学 | A kind of graphene bismuth molybdate sodium nano composite material and its preparation method and application |
| CN105879855B (en) * | 2016-04-27 | 2019-05-03 | 武汉工程大学 | A kind of graphene-γ-bismuth molybdate nanocomposite and its preparation method and application |
| CN107032401A (en) * | 2017-05-27 | 2017-08-11 | 武汉工程大学 | A kind of bismuth molybdate sodium nano material and preparation method thereof |
| CN107055614A (en) * | 2017-05-27 | 2017-08-18 | 武汉工程大学 | A kind of bismuth molybdate potassium nano material and preparation method thereof |
| CN108213453A (en) * | 2018-01-25 | 2018-06-29 | 叶剑 | A kind of preparation method of more metal nano materials |
| CN109911937A (en) * | 2019-02-01 | 2019-06-21 | 渤海大学 | A kind of NaRE (MoO4)2From sacrifice method for preparing template |
| CN109911937B (en) * | 2019-02-01 | 2021-01-22 | 渤海大学 | NaRE (MoO)4)2Preparation method of self-sacrifice template |
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