CN103526293A - Method of preparing cadmium tungstate nanowire by microwave method - Google Patents
Method of preparing cadmium tungstate nanowire by microwave method Download PDFInfo
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- CN103526293A CN103526293A CN201310477776.8A CN201310477776A CN103526293A CN 103526293 A CN103526293 A CN 103526293A CN 201310477776 A CN201310477776 A CN 201310477776A CN 103526293 A CN103526293 A CN 103526293A
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Abstract
The invention discloses a method of preparing a cadmium tungstate nanowire by a microwave method. The method comprises the following steps: respectively preparing sodium tungstate and cadmium chloride into liquor, and carrying out suction filtration after stirring; and enabling precipitates to react under action of microwaves to obtain the cadmium tungstate nanowire. The cadmium tungstate nanowire obtained by the method disclosed by the invention has the advantages of being greater in nanocrystal slenderness ratio, high in purity, excellent in luminescence property, and simple in process, quick and efficient, low in cost, environment-friendly, easy for industrialization, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of cadmium tungstate nano wire, relate in particular to a kind of method of preparing cadmium tungstate nano wire by microwave method.
Background technology
Cadmium tungstate (CdWO
4) nanocrystal has scheelite-type structure, large to x gamma ray absorption coefficient, radiation length is short, damage-resistant can be strong, be a kind of very important scintillator material, under action of ultraviolet light, can send light blue extremely yellow spectrum, therefore in the photoelectric materials such as fluorescence and laser, play an important role, at aspects such as photodiode, super large screen displayings, be used widely, especially aspect the quick components and parts of device, there is very wide application space colour development material and off-color material aspect.
At present, the existing preparation method of cadmium tungstate nano wire adopts hydrothermal method, by adding organic surface active agent, make cadmium tungstate crystal oriented growth, thereby obtain cadmium tungstate nano wire, yet this method is complex process not only, and use a large amount of organic surface active agents, environment is caused to a large amount of pollutions, and the length-to-diameter ratio of resulting cadmium tungstate nano wire is also less, can make like this luminescent properties and the damage-resistant of cadmium tungstate nano wire reduce, thereby not reach user's service requirements.
Summary of the invention
The object of the invention is in order to solve the problems of the technologies described above the deficiency of existence, provide that a kind of cadmium tungstate nanocrystal length-to-diameter ratio is large, purity is high, luminescent properties is excellent and technique simply, rapidly and efficiently, the preparation method low-cost, environmental protection is easy to suitability for industrialized production cadmium tungstate nano wire.
Cadmium tungstate the fabricate of nanowires method of the present invention, concrete steps are as follows:
Step 1, by sodium wolframate wiring solution-forming, the WO in solution
4 2-the concentration of ion is 0.05 ~ 2mol/L;
Step 2, by Cadmium chloride fine powder wiring solution-forming, the Cd in solution
2+the concentration of ion is 0.05 ~ 2mol/L;
The water-soluble liquid-phase mixing of Cadmium chloride fine powder that step 3, the sodium wolframate aqueous solution that step 1 is made and step 2 make, wherein the mol ratio of sodium wolframate and Cadmium chloride fine powder is 1:1, by after the solution stirring 10-30 obtaining minute, carries out suction filtration;
Step 4, the precipitation that step 3 is made are placed in corundum crucible, then corundum crucible is placed in the container that carbon dust is housed, and carbon dust is enclosed in around corundum crucible, and cover lid, moves to container in microwave oven;
Step 5, under the effect of microwave, react 10～90 minutes, the power of microwave oven is 160W～1000W;
After step 6, reaction finish, take out container, the standing room temperature that is cooled to, obtains well-crystallized's cadmium tungstate nano wire.
Described sodium wolframate and the purity of Cadmium chloride fine powder are all not less than chemical pure.
It is 1:1 that sodium wolframate of the present invention and Cadmium chloride fine powder proportioning are strict controlled in mol ratio, can make like this reaction meeting more abundant, thereby obtains cadmium tungstate nanocrystal good crystallinity, and purity is also very high.
In the present invention, the WO in sodium wolframate
4 2-the concentration of ion is 0.05mol/L, the Cd in Cadmium chloride fine powder
2+the concentration of ion is 0.05mol/L, and the various best performances of cadmium tungstate nano wire that obtain are different, there will be a peak-peak.
In step 3, used suction filtration technique, in step 4, crucible is placed in the container that carbon dust is housed, this is because carbon dust belongs to polar molecule, can absorb microwave, can make cadmium tungstate precursor reach the effect of crystallization, therefore in this reaction system, do not need water to absorb microwave, this just can filter water, sodium ion, chlorion in cadmium tungstate precursor precipitation solution by suction filtration technique, can obtain like this cadmium tungstate nanocrystal that purity is higher.
In the present invention, used microwave preparation technology except thering is the effect of heating, also because cadmium tungstate itself has weak polarity, also can absorb microwave simultaneously, under the effect of microwave, cadmium tungstate precursor can be rapidly heated within the extremely short time, obtains the better cadmium tungstate nanocrystal of crystallinity; In addition, microwave has the effect of guiding to the growth of cadmium tungstate crystal, thereby make cadmium tungstate crystal generation oriented growth, finally can obtain having the cadmium tungstate nano wire of one-dimentional structure, the length-to-diameter ratio of cadmium tungstate nano wire surpasses 50, and one-dimentional structure is because having very large specific surface area and length-to-diameter ratio, the performances such as its luminescent properties, damage-resistant energy can be significantly improved.Nano wire is a kind of nanoscale wire that 100 nanometers are following, have one-dimentional structure that longitudinally do not have to limit, be laterally limited in, an important component part as nanotechnology, nano wire has the more excellent performance of ratio nano sphaerocrystal, therefore, cadmium tungstate nano wire of the present invention has unique one-dimentional structure, than the sphaerocrystal of being prepared by other preparation methods, has more excellent performance and more wide application space.
The cadmium tungstate nano wire being made by microwave method have that cadmium tungstate nanocrystal length-to-diameter ratio is large, purity is high, luminescent properties is excellent and technique simply, rapidly and efficiently, low-cost, environmental protection is easy to the advantages such as suitability for industrialized production.Cadmium tungstate nano wire of the present invention has a wide range of applications at aspects such as fluorescence, photodiode, super large screen displaying, the quick components and parts of device, colour development material and off-color materials.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of cadmium tungstate nano wire of the present invention.
Fig. 2 is transmission electron microscope (TEM) photo of cadmium tungstate nano wire of the present invention.
Embodiment
Below in conjunction with example, further illustrate the present invention.
Embodiment 1
Step 1 is sodium wolframate wiring solution-forming, the WO in regulator solution
4 2-the concentration of ion is 0.05mol/L;
Step 2 is Cadmium chloride fine powder wiring solution-forming, the Cd in regulator solution
2+the concentration of ion is 0.05mol/L;
The water-soluble liquid-phase mixing of Cadmium chloride fine powder that the sodium wolframate aqueous solution that step 3 makes step 1 and step 2 make, wherein the mol ratio of sodium wolframate and Cadmium chloride fine powder is 1:1, and the solution stirring obtaining, after 10 minutes, is carried out to suction filtration;
The precipitation that step 4 makes step 3 is placed in corundum crucible, then corundum crucible is placed in the container that carbon dust is housed, and carbon dust is enclosed in around corundum crucible, cover lid, and container is moved in microwave oven;
The power of step 5 microwave oven is 160W, reacts 90 minutes under the effect of microwave;
After step 6 reaction finishes, take out reaction vessel, the standing room temperature that is cooled to, obtains well-crystallized's cadmium tungstate nano wire.Resulting is cadmium tungstate nano wire, and diameter is 20-30nm, and length is 2um-3um, and its XRD figure spectrum is shown in Fig. 1; Transmission electron microscope picture is shown in Fig. 2.
Fig. 1 illustrates that cadmium tungstate nano wire of the present invention does not have dephasign, and purity is very high, and diffraction peak is very sharp-pointed, thereby cadmium tungstate crystal good crystallinity; Fig. 2 illustrates cadmium tungstate nano wire of the present invention, and diameter is 20-30nm, and length is 2u-4u, and the length-to-diameter ratio of the cadmium tungstate nano wire obtaining surpasses 50.
Embodiment 2
Step 1 is sodium wolframate wiring solution-forming, the WO in regulator solution
4 2-the concentration of ion is 1.2mol/L;
Step 2 is Cadmium chloride fine powder wiring solution-forming, the Cd in regulator solution
2+the concentration of ion is 1.2mol/L;
The water-soluble liquid-phase mixing of Cadmium chloride fine powder that the sodium wolframate aqueous solution that step 3 makes step 1 and step 2 make, wherein the mol ratio of sodium wolframate and Cadmium chloride fine powder is 1:1, and the solution stirring obtaining, after 20 minutes, is carried out to suction filtration;
The precipitation that step 4 makes step 3 is placed in corundum crucible, then corundum crucible is placed in the container that carbon dust is housed, and carbon dust is enclosed in around corundum crucible, cover lid, and container is moved in microwave oven;
The power of step 5 microwave oven is 500W, reacts 50 minutes under the effect of microwave;
After step 6 reaction finishes, take out reaction vessel, the standing room temperature that is cooled to, obtains well-crystallized's cadmium tungstate nano wire.
Embodiment 3
Step 1 is sodium wolframate wiring solution-forming, the WO in regulator solution
4 2-the concentration of ion is 2mol/L;
Step 2 is Cadmium chloride fine powder wiring solution-forming, the Cd in regulator solution
2+the concentration of ion is 2mol/L;
The water-soluble liquid-phase mixing of Cadmium chloride fine powder that the sodium wolframate aqueous solution that step 3 makes step 1 and step 2 make, wherein the mol ratio of sodium wolframate and Cadmium chloride fine powder is 1:1, and the solution stirring obtaining, after 30 minutes, is carried out to suction filtration;
The precipitation that step 4 makes step 3 is placed in corundum crucible, then corundum crucible is placed in the container that carbon dust is housed, and carbon dust is enclosed in around corundum crucible, cover lid, and container is moved in microwave oven;
The power of step 5 microwave oven is 1000W, reacts 90 minutes under the effect of microwave;
After step 6 reaction finishes, take out reaction vessel, the standing room temperature that is cooled to, obtains well-crystallized's cadmium tungstate nano wire.
Claims (4)
1. by microwave method, prepare a method for cadmium tungstate nano wire, it is characterized in that: step 1, by sodium wolframate wiring solution-forming, the WO in solution
4 2-the concentration of ion is 0.05 ~ 2mol/L; Step 2, by Cadmium chloride fine powder wiring solution-forming, the Cd in solution
2+the concentration of ion is 0.05 ~ 2mol/L; The water-soluble liquid-phase mixing of Cadmium chloride fine powder that step 3, the sodium wolframate aqueous solution that step 1 is made and step 2 make, by after the solution stirring 10-30 obtaining minute, carries out suction filtration; Step 4, the precipitation that step 3 is made are placed in corundum crucible, then corundum crucible is placed in the container that carbon dust is housed, and carbon dust is enclosed in around corundum crucible, and cover lid, moves to container in microwave oven; Step 5, under the effect of microwave, react 10～90 minutes, the power of microwave oven is 160W～1000W; After step 6, reaction finish, take out container, the standing room temperature that is cooled to, obtains cadmium tungstate nano wire.
2. a kind of method of preparing cadmium tungstate nano wire by microwave method according to claim 1, is characterized in that: the WO in sodium tungstate solution
4 2-the concentration of ion is 0.05mol/L; Cd in cadmium chloride solution
2+the concentration of ion is 0.05mol/L.
3. a kind of method of preparing cadmium tungstate nano wire by microwave method according to claim 1, is characterized in that: the WO in sodium tungstate solution
4 2-the concentration of ion is 2mol/L; Cd in cadmium chloride solution
2+the concentration of ion is 2mol/L.
4. a kind of method of preparing cadmium tungstate nano wire by microwave method according to claim 1, is characterized in that: the mol ratio of sodium wolframate and Cadmium chloride fine powder is 1:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107010672A (en) * | 2017-05-04 | 2017-08-04 | 洛阳理工学院 | A kind of preparation method of lead tungstate nano tubular crystal |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294304A (en) * | 2007-04-29 | 2008-10-29 | 宁波大学 | Growth technique for cadmium tungstate twinkling monocrystal with crucible descent method |
| CN101538739A (en) * | 2009-04-14 | 2009-09-23 | 宁波大学 | Cadmium tungstate crystal and preparation method thereof |
| CN201504333U (en) * | 2009-08-07 | 2010-06-09 | 上海屹尧仪器科技发展有限公司 | Microwave auxiliary heating body |
| CN102358950A (en) * | 2011-10-20 | 2012-02-22 | 西安工程大学 | Preparation method of cadmium tungstate monocrystal nanoribbon |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294304A (en) * | 2007-04-29 | 2008-10-29 | 宁波大学 | Growth technique for cadmium tungstate twinkling monocrystal with crucible descent method |
| CN101538739A (en) * | 2009-04-14 | 2009-09-23 | 宁波大学 | Cadmium tungstate crystal and preparation method thereof |
| CN201504333U (en) * | 2009-08-07 | 2010-06-09 | 上海屹尧仪器科技发展有限公司 | Microwave auxiliary heating body |
| CN102358950A (en) * | 2011-10-20 | 2012-02-22 | 西安工程大学 | Preparation method of cadmium tungstate monocrystal nanoribbon |
Non-Patent Citations (3)
| Title |
|---|
| CHANG SUNG LIM,ET AL.: "Microwave-assisted synthesis of CdWO4 by solid-state metathetic reaction", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| YONGGANG WANG,ET AL.: "Controllable synthesis of CdWO4 nanorods and nanowires via a surfactant-free hydrothermal method", 《JOURNAL OF THE CERAMIC SOCIETY OF JAPAN》 * |
| 杨琳琳等: "CdWO4纳米晶形貌可控合成", 《人工晶体学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107010672A (en) * | 2017-05-04 | 2017-08-04 | 洛阳理工学院 | A kind of preparation method of lead tungstate nano tubular crystal |
| CN107010672B (en) * | 2017-05-04 | 2018-05-22 | 洛阳理工学院 | A kind of preparation method of lead tungstate nano tubular crystal |
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