CN101734721A - Method for synthesis of microemulsion of strontium molybdate nano light emitting material - Google Patents
Method for synthesis of microemulsion of strontium molybdate nano light emitting material Download PDFInfo
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- CN101734721A CN101734721A CN200910201572A CN200910201572A CN101734721A CN 101734721 A CN101734721 A CN 101734721A CN 200910201572 A CN200910201572 A CN 200910201572A CN 200910201572 A CN200910201572 A CN 200910201572A CN 101734721 A CN101734721 A CN 101734721A
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Abstract
The invention discloses a method for synthesis of microemulsion of strontium molybdate nano light emitting material, comprising the steps of preparing 0.2 mol/L strontium chloride solution and 0.2 mol/L molybdenum source solution, adding mixed solution of the n-butyl alcohol and the surfactant of ethane-di-dodecyl dimethyl ammonium bromide, n-octane and the strontium chloride solution to a container in sequence, supersonically oscillating the container, placing the container in a constant-temperature water bath until the solution in the contain being clear and transparent to obtain strontium chloride microemulsion, preparing molybdenum source microemulsion by using the molybdenum source solution rather than the strontium chloride solution with the similar method, rapidly mixing the strontium chloride microemulsion and the molybdenum source microemulsion, supersonically oscillating the strontium chloride microemulsion and the molybdenum source microemulsion until the strontium chloride microemulsion and the molybdenum source microemulsion being evenly mixing, adding acetone for demulsifing after the reaction of the strontium chloride microemulsion and the molybdenum source microemulsion, absorbing supernatant liquor, and washing the deposited products of reaction with distilled water, acetone and absolute ethyl alcohol in sequence to obtain the strontium molybdate nano emitting material which has the length of 100-600nm and the maximum width of 30-200nm and is in the structure of spindle. The method for synthesizing strontium molybdate nano emitting material microemulsion is easy to obtain the raw materials, is simple, has low cost, ensures that the product of reaction has high purity and controllable morphology and size and is suitable for the scale production.
Description
Technical field
The present invention relates to a kind of preparation method of strontium molybdate, the method for synthesis of microemulsion of a kind of nanometer strontium molybdate of more specifically saying so.
Background technology
Strontium wolframate with scheelite-type structure has the excellent flicker characteristics of luminescence, can be in field widespread uses such as high energy physics, laser acquisitions.The strontium molybdate that has same crystal structure with strontium wolframate also can be used as the use of flicker twinkler.
The research report of existing strontium molybdate mainly concentrates on the preparation and the luminescent properties research of micron order strontium molybdate crystalline material.In recent years, some researchers have prepared the nanometer strontium molybdate by methods such as hydrothermal method and solvent-thermal methods.Hydrothermal method has higher synthetic yield, and products obtained therefrom purity height is easy to large-scale production, but has the problem of product cut size excessive (submicron).Though solvent-thermal method can obtain the nano level product,, thereby greatly influence product purity because of the introducing of organic solvent makes that the last handling process of product is very loaded down with trivial details.Therefore develop a kind of simple to operate, with low cost, reaction conditions is gentle, optical property is excellent, the method that is easy to the large-scale production strontium molybdate nano light emitting material is significant.
Summary of the invention
Technical problem to be solved by this invention provide a kind of with low cost, optical property is excellent, the method for synthesis of microemulsion of convenient post-treatment, the strontium molybdate nano light emitting material that is produced on a large scale.
The technical solution used in the present invention
A kind of method for synthesis of microemulsion of strontium molybdate nano light emitting material comprises the steps:
(1), take by weighing the molybdenum source of strontium chloride and the 0.010mol of 0.010mol, then it is dissolved in the strontium chloride solution of making concentration 0.2mol/L in the 50mL distilled water and the molybdenum source solution of 0.2mol/L respectively;
Described molybdenum source is selected from Na
2MoO
4Or K
2MoO
4
(2), the strontium chloride solution that in container, adds mixed solution, octane and step (1) gained of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol successively, ultrasonic 15min under power 100W, with being placed on constant temperature 30min in 35 ℃ of water-baths, to the solution clear, make the microemulsion of strontium chloride;
The mass ratio of tensio-active agent and propyl carbinol is 1: 1 in the mixed solution of above-mentioned ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol;
The strontium chloride solution of mixed solution, octane and step (1) gained of above-mentioned ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol by volume, i.e. the mixed solution of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol: octane: the strontium chloride solution of step (1) gained is 2～5: 5～8: 0.5～1.5;
(3), the molybdenum source solution that in container, adds mixed solution, octane and step (1) gained of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol successively, ultrasonic 15min under power 100W, with being placed on constant temperature 30min in 35 ℃ of water-baths, to the solution clear, make the microemulsion in molybdenum source;
The mass ratio of ethane in the mixed solution of above-mentioned ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol is 1: 1;
The molybdenum source solution of mixed solution, octane and step (1) gained of above-mentioned ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol by volume, i.e. the mixed solution of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol: octane: the molybdenum source solution of step (1) gained is 2～5: 5～8: 0.5～1.5;
(4), the microemulsion in the microemulsion of the strontium chloride that step (2) and step (3) is prepared and molybdenum source mixes, and behind ultrasonic 10min under the 100W power, reaction 2～8h adds 20mL acetone breakdown of emulsion again, after using whizzer with the centrifugal 10min of the rotating speed of 200rpm/min subsequently, inhale and remove supernatant liquid;
(5), precipitated product that centrifugation is obtained respectively cleans three times with acetone, distilled water and dehydrated alcohol successively, promptly gets strontium molybdate nano light emitting material of the present invention.
Product strontium molybdate nano light emitting material of the present invention, length are that 100～600nm, the widest part are the spindle-shaped structure of 30～200nm, are stored in the dehydrated alcohol.
In the method for synthesis of microemulsion of strontium molybdate nano light emitting material, owing in strontium chloride and molybdenum source, introduce efficient ethane-didodecyldimethylammbromide bromide tensio-active agent, can induce the end product nanometer strontium molybdate of synthetic different-shape and size, and the fluorescence peak blue shift degree of product increases.
The beneficial effect of the invention
Because the present invention is the micro emulsion synthetic system, utilize the formed reverse latex system of ethane-didodecyldimethylammbromide bromide tensio-active agent and octane to realize the control growing of appearance of nano material and size, synthesize strontium molybdate nano light emitting material, for the technology of preparing of nano material is had laid a good foundation with good pattern.
Because the present invention only need adjust the concentration, micro emulsion generated time of kind, the microemulsion of reactant etc., get final product synthetic yield up to nanometer strontium molybdate 90%, that pattern is different, optical property is excellent, the strontium molybdate nano light emitting material of gained, length are that 100～600nm, the widest part are the spindle-shaped structure of 30～200nm.
The product of the present invention's preparation has the good flicker characteristics of luminescence: the emission peak blue shift.
The constructed method for synthesis of microemulsion of the present invention is simple, with low cost, the product purity height, and optical property is good, convenient post-treatment, is fit to the industrialization operation, and new approach is provided for the control of nano material is synthetic.
Description of drawings
Scanning electronic microscope (SEM) photo of Fig. 1, embodiment 1 product.
Embodiment
Also in conjunction with the accompanying drawings the present invention is described in further detail below by embodiment, but do not limit the present invention.
Embodiment 1
(1), take by weighing the strontium chloride of 0.010mol and the Sodium orthomolybdate of 0.010mol, then it is dissolved in strontium chloride and the sodium molybdate solution of making concentration 0.2mol/L in the 50mL distilled water respectively;
(2), add the strontium chloride solution that mixed solution (mass ratio is 1: 1), octane and the first step of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol make successively according to 3: 7: 1 mass ratio, ultrasonic 15min under power 100W, with being placed on constant temperature 30min in 35 ℃ of water-baths, to the solution clear, make the microemulsion of strontium chloride.Replace strontium chloride solution with the prepared sodium molybdate solution of the first step, adopt similar methods to obtain the Sodium orthomolybdate microemulsion.Then two kinds of prepared micellar solutions are mixed rapidly, and ultrasonic 10min mixes it under 100W power.Behind the question response 4h, add the acetone breakdown of emulsion.Centrifugal with whizzer with the rotating speed of 200rpm/min, supernatant liquid glue head dropper sucking-off;
(3), precipitated product that centrifugation is obtained cleans (each is three times) with acetone, distilled water and dehydrated alcohol successively, can obtain product of the present invention.
Use scanning electronic microscope (SEM) and X-ray powder diffraction (XRD) that the pattern and the structure of product are characterized respectively.
As can be seen from Fig. 1, SEM shows that product is the spindle-shaped structure of long 350nm, wide 70nm.
Contrast by the JCPDS card of XRD figure spectrum, can confirm that product is pure, be the strontium molybdate of scheelite-type structure with standard.
Fluorescent spectroscopy is the result show, product has the good flicker characteristics of luminescence.
Embodiment 2
Choose 2: 8: 1 mass ratio, other conditions and step and embodiment 1 are identical, and products therefrom is the nanometer spindle of long 200nm, wide 75nm.Product has the crystalline structure identical with embodiment 1.Its purity height, degree of crystallinity is good.Compare the fluorescence emission peak blue shift of product with embodiment 1.
Embodiment 3
Choose 5: 5: 1 mass ratio, other conditions and step and embodiment 1 are identical, and the product that obtains is the accurate nanometer spindle of long 500nm, wide 200nm.Product has the crystalline structure identical with embodiment 1.Its purity height, degree of crystallinity is good.Compare with embodiment 1, the fluorescence peak blue shift degree of product is less.
Embodiment 4
Choose 3: 7: 1.5 mass ratio, other conditions and step and embodiment 1 are identical, and products therefrom is the accurate nanometer spindle of long 400nm, wide 150nm.The crystallographic system of product is identical with embodiment 1, the product purity height, and degree of crystallinity and optical property are good.Compare with embodiment 1, the blue shift degree of fluorescence peak reduces.
Embodiment 5
Choose 3: 7: 0.5 mass ratio, change Sodium orthomolybdate into potassium molybdate, the reaction times changes 2 hours into, and other conditions and step and embodiment 1 are identical, and the product that obtains is the nanometer spindle of long 100nm, wide about 30nm, and the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity and optical property are good.Compare with embodiment 1, the blue shift degree of fluorescence peak increases.
Embodiment 6
Choose 4: 6: 1 mass ratio, change Sodium orthomolybdate into potassium molybdate, the reaction times changes 2 hours into, and other conditions and step and embodiment 1 are identical, and the product that obtains is the nanometer spindle of long 100nm, wide about 30nm, and the crystallographic system of product is identical with embodiment 1.The product purity height, degree of crystallinity and optical property are good.Compare with embodiment 1, the blue shift degree of fluorescence peak increases.
Embodiment 7
Choose 3: 7: 0.5 mass ratio, change Sodium orthomolybdate into potassium molybdate, the reaction times changes 8 hours into, and other conditions and step and embodiment 1 are identical, and obtained product is the accurate nanometer spindle of long 600nm, wide about 200nm, and the crystallographic system of product is identical with embodiment 1.Its purity height, degree of crystallinity and optical property are good.Compare with embodiment 1, the blue shift degree of fluorescence peak reduces.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (4)
1. the method for synthesis of microemulsion of a strontium molybdate nano light emitting material is characterized in that comprising the following steps:
(1), take by weighing the molybdenum source of strontium chloride and the 0.010mol of 0.010mol, then it is dissolved in the strontium chloride solution of making concentration 0.2mol/L in the 50mL distilled water and the molybdenum source solution of 0.2ol/L respectively;
Described molybdenum source is selected from Na
2MoO
4Or K
2MoO
4
(2), the strontium chloride solution that in container, adds mixed solution, octane and step (1) gained of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol successively, ultrasonic 15min under power 100W, with being placed on constant temperature 30min in 35 ℃ of water-baths, to the solution clear, make the microemulsion of strontium chloride;
The mass ratio of ethane in the mixed solution of above-mentioned ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol is 1: 1;
The strontium chloride solution of mixed solution, octane and step (1) gained of above-mentioned ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol is pressed mass ratio, i.e. the mixed solution of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol: octane: the strontium chloride solution of step (1) gained is 2～5: 5～8: 0.5～1.5;
(3), the molybdenum source solution that in container, adds mixed solution, octane and step (1) gained of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol successively, ultrasonic 15min under power 100W, with being placed on constant temperature 30min in 35 ℃ of water-baths, to the solution clear, make the microemulsion in molybdenum source;
The mass ratio of ethane in the mixed solution of above-mentioned ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol is 1: 1;
The molybdenum source solution of mixed solution, octane and step (1) gained of above-mentioned ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol is pressed mass ratio, i.e. the mixed solution of ethane-didodecyldimethylammbromide bromide tensio-active agent and propyl carbinol: octane: the molybdenum source solution of step (1) gained is 2～5: 5～8: 0.5～1.5;
(4), the microemulsion in the microemulsion of the strontium chloride that step (2) and step (3) is prepared and molybdenum source mixes, and behind ultrasonic 10min under the 100W power, reaction 2～8h adds 20mL acetone breakdown of emulsion again, after using whizzer with the centrifugal 10min of the rotating speed of 200rpm/min subsequently, inhale and remove supernatant liquid;
(5), precipitated product that centrifugation is obtained respectively cleans three times with acetone, distilled water and dehydrated alcohol successively, promptly gets strontium molybdate nano light emitting material of the present invention.
2. according to the method for synthesis of microemulsion of the described strontium molybdate nano light emitting material of claim 1, it is characterized in that the micro emulsion synthetic system in the step (2) has been introduced ethane-didodecyldimethylammbromide bromide tensio-active agent.
3. according to the method for synthesis of microemulsion of the described strontium molybdate nano light emitting material of claim 1, it is characterized in that the strontium molybdate nano light emitting material of gained in the step (5) is the spindle shape.
4. the strontium molybdate nano light emitting material of gained according to the method for synthesis of microemulsion of the described strontium molybdate nano light emitting material of claim 3, is characterized in that the strontium molybdate nano light emitting material of spindle shape shape, and length is that 100～600nm, the widest part are 30～200nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105984902A (en) * | 2016-02-19 | 2016-10-05 | 安徽大学 | Preparation method of strontium-molybdate-dopable nano material |
| CN106915773A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of strontium molybdate skeleton |
-
2009
- 2009-12-22 CN CN200910201572A patent/CN101734721A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105984902A (en) * | 2016-02-19 | 2016-10-05 | 安徽大学 | Preparation method of strontium-molybdate-dopable nano material |
| CN105984902B (en) * | 2016-02-19 | 2018-06-29 | 安徽大学 | A kind of strontium molybdate nano material preparation method adulterated |
| CN106915773A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of strontium molybdate skeleton |
| CN106915773B (en) * | 2017-05-04 | 2018-03-06 | 洛阳理工学院 | A kind of preparation method of strontium molybdate skeleton |
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Open date: 20100616 |