CN107384389A - A kind of preparation method of calcium molybdate/molybdenum disulfide composite luminescent material - Google Patents
A kind of preparation method of calcium molybdate/molybdenum disulfide composite luminescent material Download PDFInfo
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- CN107384389A CN107384389A CN201710582333.3A CN201710582333A CN107384389A CN 107384389 A CN107384389 A CN 107384389A CN 201710582333 A CN201710582333 A CN 201710582333A CN 107384389 A CN107384389 A CN 107384389A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
- C09K11/681—Chalcogenides
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Abstract
The invention discloses a kind of preparation method of calcium molybdate/molybdenum disulfide composite luminescent material, concretely comprise the following steps：0.85g sodium molybdates are dissolved in 30mL water and stir 5min formation sodium molybdate aqueous solutions, sodium molybdate aqueous solution is poured into polytetrafluoroethyllining lining, two egg shells are put into water and soaked, the inner membrance that then will be attached on egg shell, which is removed, to be put into sodium molybdate aqueous solution；Polytetrafluoroethyllining lining is put into reactor, it is placed in after sealing in drying box and reacts 24h in 160 240 DEG C, pass through deionized water and washes of absolute alcohol to neutrality after product is taken out, then calcium molybdate/molybdenum disulfide composite luminescent material is obtained in 40 DEG C of dry 6 48h, the composite luminescent material sends blue light and green glow under ultraviolet excitation.The present invention first passage on the premise of not introducing rare earth element with molybdenum disulfide is compound realize blue light and green glow while launch, synthesis technique is simpler and cost is cheap.
Description
Technical field
The invention belongs to the synthesis technical field of embedded photoluminescent material, and in particular to a kind of calcium molybdate/molybdenum disulfide is compound
The preparation method of luminescent material.
Background technology
China's Mo resource rich content, molybdate is the most important colony of molybdenum compound, indispensable in high-tech area, is opened
Hair molybdic acid salt material has important economic value and social value.Molybdate is a kind of effective catalyst, ion conductor and surpassed
Conductor, it is widely used in preparing optical fiber, magnetic material, catalysis material and humidity sensor etc., especially has white
The molybdate of tungsten ore structure, in field of light emitting materials（Such as laser, scintillator, light emitting diode）It is widely used.In recent years, respectively
State's researcher more and more pays close attention to functional molybdate material, and outstanding work is made that in terms of molybdate is synthesized.
Calcium molybdate（CaMoO4）It is a kind of important embedded photoluminescent material, heat endurance and chemical stability are good, are simultaneously
A kind of luminescent material acceptor well.Single calcium molybdate mainly produces green glow after exciting, and in order to realize white light LEDs, need
Want luminescent material while produce red, blue, green three coloured light.Meanwhile in order to obtain high lumen output, the half-peak breadth of emission spectra will be use up
Measure it is narrow, and individually calcium molybdate green spectrum it is very wide.In order to realize the transmitting of red light and blue light, research at present is main to concentrate
On rare earth ion doped, the rare earth ion of doping has：Eu3+、Tb3+、Dy3+Deng.In numerous methods of synthesizing luminescent material,
High temperature solid-state method is a kind of most widely used, the better simply synthetic method of technique, but high sintering temperature can cause MoO3Wave
Hair causes the uneven of compound.Liquid phase method is widely used in regulation and control substance pattern, including hydro-thermal method, solvent-thermal method, microwave method
With surfactant method etc., wherein hydro-thermal method can directly obtain dispersiveness and the good powder of crystallinity, it is not necessary at high temperature
Reason, it is not necessary to add organic activating agent and template, phenomena such as product caused by avoiding powder reuniting and organic matter is impure.It is dilute
Soil, which adulterates, makes calcium molybdate produce feux rouges and green glow after exciting, and research is extensive, and multiple by the compound preparation of calcium molybdate and other materials
The research for closing luminescent material is rarely reported.
The content of the invention
Present invention solves the technical problem that it there is provided a kind of preparation side of calcium molybdate/molybdenum disulfide composite luminescent material
Method, this method first passage on the premise of not introducing rare earth element with molybdenum disulfide is compound realize blue light and green glow while
Transmitting, synthesis technique is simpler and cost is cheap.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, a kind of calcium molybdate/molybdenum disulfide recombination luminescence
The preparation method of material, it is characterised in that concretely comprise the following steps：
（1）0.85g sodium molybdates are dissolved in 30mL water and stir 5min formation sodium molybdate aqueous solutions, sodium molybdate aqueous solution are poured into poly-
In tetrafluoroethene liner, two egg shells are put into water and soaked, the inner membrance that then will be attached on egg shell, which is removed, is put into molybdenum
In acid sodium aqueous solution；
（2）Polytetrafluoroethyllining lining is put into reactor, is placed in after sealing in drying box and reacts 24h in 160-240 DEG C, will produced
After thing taking-up then calcium molybdate/curing is obtained in 40 DEG C of dry 6-48h to neutrality by deionized water and washes of absolute alcohol
Molybdenum composite luminescent material, the composite luminescent material send blue light and green glow under ultraviolet excitation.
The present invention has synthesized composite luminescent material calcium molybdate/molybdenum disulfide powder first, compared with conventional method, with egg
Shell inner membrance is that raw material can effectively be applied to traditional food refuse egg shell, and realization is turned waste into wealth, the recombination luminescence material
Material sends blue light and green glow under ultraviolet excitation, compared with single calcium molybdate can only send wide spectrum green glow, the compound hair
The blue emission spectrum of luminescent material is narrow, and green spectrum is more concentrated, and has high lumen output, and it can be used for the preparation of luminescent device,
Have a wide range of applications scope.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of calcium molybdate made from embodiment 1-3/molybdenum disulfide composite luminescent material；
Fig. 2 is the SEM figures of calcium molybdate made from embodiment 1-3/molybdenum disulfide composite luminescent material；
Fig. 3 is the luminescence generated by light curve of calcium molybdate made from embodiment 1-3/molybdenum disulfide composite luminescent material（Excitation wavelength
254nm）.
Embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
By 0.85g sodium molybdates（Na2MoO4）It is dissolved in 30mL water, stirring 5min forms sodium molybdate aqueous solution, and sodium molybdate is water-soluble
Liquid pours into polytetrafluoroethyllining lining, and two egg shells are put into water and soaked, the inner membrance that then will be attached on egg shell is removed
It is put into sodium molybdate aqueous solution；Polytetrafluoroethyllining lining is put into reactor, is placed in after sealing in drying box in 160 DEG C of reactions
24h, after product is taken out then brown molybdenum is obtained in 40 DEG C of dry 12h to neutrality by deionized water and washes of absolute alcohol
Sour calcium/molybdenum disulfide composite luminescent material, composite luminescent material is put into XRF and tests its luminosity, excitation wave
Long 254nm, show obvious blue light and green emission.
Embodiment 2
By 0.85g sodium molybdates（Na2MoO4）It is dissolved in 30mL water, stirring 5min forms sodium molybdate aqueous solution, and sodium molybdate is water-soluble
Liquid pours into polytetrafluoroethyllining lining, and two egg shells are put into water and soaked, the inner membrance that then will be attached on egg shell is removed
It is put into sodium molybdate aqueous solution；Polytetrafluoroethyllining lining is put into reactor, is placed in after sealing in drying box in 200 DEG C of reactions
24h, after product is taken out then brownish black is obtained in 40 DEG C of dry 12h to neutrality by deionized water and washes of absolute alcohol
Calcium molybdate/molybdenum disulfide composite luminescent material, composite luminescent material is put into XRF and tests its luminosity, is excited
Wavelength 254nm, show obvious blue light and green emission.
Embodiment 3
By 0.85g sodium molybdates（Na2MoO4）It is dissolved in 30mL water, stirring 5min forms sodium molybdate aqueous solution, and sodium molybdate is water-soluble
Liquid pours into polytetrafluoroethyllining lining, and two egg shells are put into water and soaked, the inner membrance that then will be attached on egg shell is removed
It is put into sodium molybdate aqueous solution；Polytetrafluoroethyllining lining is put into reactor, is placed in after sealing in drying box in 240 DEG C of reactions
24h, after product is taken out then black molybdenum is obtained in 40 DEG C of dry 12h to neutrality by deionized water and washes of absolute alcohol
Sour calcium/molybdenum disulfide composite luminescent material, composite luminescent material is put into XRF and tests its luminosity, excitation wave
Long 254nm, show obvious blue light and green emission.
Embodiment above describes the general principle of the present invention, main features and advantages, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (1)
1. the preparation method of a kind of calcium molybdate/molybdenum disulfide composite luminescent material, it is characterised in that concretely comprise the following steps：
（1）0.85g sodium molybdates are dissolved in 30mL water and stir 5min formation sodium molybdate aqueous solutions, sodium molybdate aqueous solution are poured into poly-
In tetrafluoroethene liner, two egg shells are put into water and soaked, the inner membrance that then will be attached on egg shell, which is removed, is put into molybdenum
In acid sodium aqueous solution；
（2）Polytetrafluoroethyllining lining is put into reactor, is placed in after sealing in drying box and reacts 24h in 160-240 DEG C, will produced
After thing taking-up then calcium molybdate/curing is obtained in 40 DEG C of dry 6-48h to neutrality by deionized water and washes of absolute alcohol
Molybdenum composite luminescent material, the composite luminescent material send blue light and green glow under ultraviolet excitation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109663590A (en) * | 2018-12-29 | 2019-04-23 | 泉州师范学院 | It is a kind of using egg shell as catalysis material of reactor and the preparation method and application thereof |
| CN110040779A (en) * | 2019-05-05 | 2019-07-23 | 河南师范大学 | A kind of preparation method of calcium molybdate luminescent material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109663590A (en) * | 2018-12-29 | 2019-04-23 | 泉州师范学院 | It is a kind of using egg shell as catalysis material of reactor and the preparation method and application thereof |
| CN110040779A (en) * | 2019-05-05 | 2019-07-23 | 河南师范大学 | A kind of preparation method of calcium molybdate luminescent material |
| CN110040779B (en) * | 2019-05-05 | 2021-07-13 | 河南师范大学 | Preparation method of calcium molybdate luminescent material |
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