CN104087289B - A kind of method utilizing waste silicon powder water heat transfer nanometer zinc silicate luminescent material - Google Patents

A kind of method utilizing waste silicon powder water heat transfer nanometer zinc silicate luminescent material Download PDF

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CN104087289B
CN104087289B CN201410306154.3A CN201410306154A CN104087289B CN 104087289 B CN104087289 B CN 104087289B CN 201410306154 A CN201410306154 A CN 201410306154A CN 104087289 B CN104087289 B CN 104087289B
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silicon powder
luminescent material
zinc silicate
waste silicon
silicate luminescent
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CN104087289A (en
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温福山
王燕
王维
杜永霞
燕友果
张军
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China University of Petroleum East China
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China University of Petroleum East China
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Abstract

The invention discloses a kind of method utilizing waste silicon powder water heat transfer nanometer zinc silicate luminescent material, the concrete steps of described method are as follows: (1) is by Zn (CH 3cOO) 22H 2o, Mn (NO 3) 24H 2o and cetyl trimethylammonium bromide are dissolved in deionized water, then add waste silicon powder, and stirring 15min, then adds sodium hydroxide or concentration is the ammoniacal liquor of 25%, stirs 10min, obtains mixing solutions; (2) mixing solutions prepared by step (1) is put into the reactor that liner is tetrafluoroethylene, reactor is sealed, put into the baking oven reaction 12-48h that temperature is 130-200 DEG C, then room temperature is naturally cooled to after taking out, by product distilled water wash, centrifugation, obtains zinc silicate luminescent material after seasoning.Method of the present invention is raw material with waste silicon powder, expands the scope of reactant, can make full use of industrial waste, reaches the object of resource recycling, and method of the present invention is hydro-thermal single step reaction, and method is simple, and energy consumption is low.

Description

A kind of method utilizing waste silicon powder water heat transfer nanometer zinc silicate luminescent material
Technical field
The present invention relates to Inorganic synthese technical field, particularly relate to a kind of method utilizing waste silicon powder water heat transfer nanometer zinc silicate luminescent material.
Background technology
Fluorescent material to be coordinated with trace active agent by metal (zinc, chromium) sulfide or rare earth oxide to form through calcining.Colourless or shallow white, is under UV-light (200 ~ 400nm) is irradiated, according to the difference of metal in material and activator species, content, and presents the visible ray (400 ~ 800nm) of shades of colour.
Inorganic fluorescent material be represented as rare earth luminescence and rare-earth luminescent material, its advantage is that receptivity is strong, and turnover ratio is high, and the narrowband emission of rare earth compounding central ion is conducive to total colouring, and physicochemical property are stablized.Because rare earth ion has abundant energy level and 4f transition of electron characteristic, make rare earth become luminous treasure-house, for high-tech area particularly field of information communication provide the luminescent material of superior performance.Common inorganic fluorescent material is with the sulfide of alkaline-earth metal (as ZnS, CaS) aluminate (SrAl 2o 4, CaAl 2o 4, BaAl 2o 4) etc. as luminous host, using rare earth lanthanide [europium (Eu), samarium (Sm), erbium (Er), neodymium (Nd) etc.] as activator and co-activator.
The traditional preparation methods of inorganic phosphor is high temperature solid-state method, but along with the quick renewal of new technology, the raising of luminescent material performance index needs to overcome the intrinsic defect of classical synthetic method, some new methods are arisen at the historic moment, as combustion method, sol-gel processing, hydrothermal deposition method, microwave method etc.
Zinc silicate is as a kind of luminescent material, of many uses, its industrial process is high temperature solid-state method, there is patent report hydrothermal synthesis method, but the general reaction raw materials adopted is silicate and zinc salt (CN102502672A: a kind of layered multi-stage zinc silicate and preparation method thereof and apply), or amorphous nano silicon-dioxide and zinc salt (CN102976344A: a kind of preparation method of zinc silicate nanometer material).But it is narrow mostly to there is reactant in existing synthetic method, the shortcoming of reaction method complexity.
Summary of the invention
The invention provides a kind of method utilizing waste silicon powder water heat transfer nanometer zinc silicate luminescent material.
The present invention adopts following technical scheme:
The present invention utilizes the concrete steps of the method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material as follows:
(1) by Zn (CH 3cOO) 22H 2o, Mn (NO 3) 24H 2o and cetyl trimethylammonium bromide are dissolved in deionized water, Zn (CH 3cOO) 22H 2o, Mn (NO 3) 24H 2the weight ratio of O and cetyl trimethylammonium bromide is 3-6:0.01-0.03:0.05, and the weightmeasurement ratio of cetyl trimethylammonium bromide and deionized water is 0.05:40-60g/ml, then adds waste silicon powder, waste silicon powder and Zn (CH 3cOO) 22H 2the weight ratio of O is 0.3-0.7:3-6, and stirring 15min, then adds sodium hydroxide or concentration is the ammoniacal liquor of 25%, stirs 10min, obtains mixing solutions;
(2) mixing solutions prepared by step (1) is put into the reactor that liner is tetrafluoroethylene, reactor is sealed, put into the baking oven reaction 12-48h that temperature is 130-200 DEG C, then room temperature is naturally cooled to after taking out, by product distilled water wash, centrifugation, obtains zinc silicate luminescent material after seasoning.
In step (1), Zn (CH 3cOO) 22H 2o, Mn (NO 3) 24H 2the weight ratio of O and cetyl trimethylammonium bromide is preferably 4.65:0.01:0.05.
In step (1), the weightmeasurement ratio of cetyl trimethylammonium bromide and deionized water is preferably 0.05:50g/ml.
In step (1), waste silicon powder and Zn (CH 3cOO) 22H 2the weight ratio of O is preferably 0.56:4.65.
In step (1), the weight ratio of sodium hydroxide and cetyl trimethylammonium bromide is 0.01:0.05.
In step (1), concentration is the ammoniacal liquor of 25% and the weight ratio of cetyl trimethylammonium bromide is 0.20:0.05.
In step (2), preferably put into the baking oven reaction 48h that temperature is 130 DEG C.
Positively effect of the present invention is as follows:
The present invention utilizes the method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material to take waste silicon powder as raw material, expand the scope of reactant, industrial waste-silica flour can be made full use of, reach the object of resource recycling, and method of the present invention is hydro-thermal single step reaction, method is simple, and energy consumption is low, and industrial high temperature solid-state method can be replaced to carry out synthetic silicic acid zinc.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction spectrogram of zinc silicate luminescent material prepared by embodiment 1.
Fig. 2 is the luminescent spectrum figure of zinc silicate luminescent material prepared by embodiment 1.
Fig. 3 is the transmission electron microscope photo of zinc silicate luminescent material prepared by embodiment 1.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1
By 4.65gZn (CH 3cOO) 22H 2o, 0.01gMn (NO 3) 24H 2o, 0.05g cetyl trimethylammonium bromide, be dissolved in 50 ml deionized water, add 0.56g waste silicon powder, stir 15 minutes, then 0.01gNaOH is added, stir 10 minutes, said mixture being transferred to liner is in 100 milliliters of reactors of tetrafluoroethylene, is sealed by reactor, put into temperature be 130 DEG C baking oven reaction 48 hours, take out naturally cooling, by product distilled water wash, centrifugation, obtain zinc silicate luminescent material 4.22g after seasoning, product is green under 254nm ultraviolet excitation.
Embodiment 2
By 4.60gZn (CH 3cOO) 22H 2o, 0.02gMn (NO 3) 24H 2o, 0.05g cetyl trimethylammonium bromide, be dissolved in 50 ml deionized water, add 0.56g waste silicon powder, stir 15 minutes, then 0.01gNaOH is added, stir 10 minutes, said mixture being transferred to liner is in 100 milliliters of reactors of tetrafluoroethylene, is sealed by reactor, put into temperature be 130 DEG C baking oven reaction 48 hours, take out naturally cooling, by product distilled water wash, centrifugation, obtain zinc silicate luminescent material 4.20g after seasoning, product is green under 254nm ultraviolet excitation.
Embodiment 3
By 4.95gZn (CH 3cOO) 22H 2o, 0.01gMn (NO 3) 24H 2o, 0.05g cetyl trimethylammonium bromide, be dissolved in 50 ml deionized water, add 0.55g waste silicon powder, stir 15 minutes, then 0.01gNaOH is added, stir 10 minutes, said mixture being transferred to liner is in 100 milliliters of reactors of tetrafluoroethylene, is sealed by reactor, put into temperature be 200 DEG C baking oven reaction 12 hours, take out naturally cooling, by product distilled water wash, centrifugation, obtain zinc silicate luminescent material 4.02g after seasoning, product is green under 254nm ultraviolet excitation.
Embodiment 4
By 5.05gZn (CH 3cOO) 22H 2o, 0.01gMn (NO 3) 24H 2o, 0.05g cetyl trimethylammonium bromide, be dissolved in 50 ml deionized water, add 0.56g waste silicon powder, stir 15 minutes, then 0.20g25% ammoniacal liquor is added, stir 10 minutes, said mixture being transferred to liner is in 100 milliliters of reactors of tetrafluoroethylene, is sealed by reactor, put into temperature be 140 DEG C baking oven reaction 48 hours, take out naturally cooling, by product distilled water wash, centrifugation, obtain zinc silicate luminescent material 4.12g after seasoning, product is green under 254nm ultraviolet excitation.
Embodiment 5
By 5.10gZn (CH 3cOO) 22H 2o, 0.01gMn (NO 3) 24H 2o, 0.05g cetyl trimethylammonium bromide, be dissolved in 50 ml deionized water, add 0.56g waste silicon powder, stir 15 minutes, then 0.20g25% ammoniacal liquor is added, stir 10 minutes, said mixture being transferred to liner is in 100 milliliters of reactors of tetrafluoroethylene, is sealed by reactor, put into temperature be 200 DEG C baking oven reaction 12 hours, take out naturally cooling, by product distilled water wash, centrifugation, obtain zinc silicate luminescent material 4.15g after seasoning, product is green under 254nm ultraviolet excitation.
Fig. 1 is the X-ray diffraction spectrogram of zinc silicate luminescent material prepared by embodiment 1, and as seen from Figure 1, zinc silicate luminescent material prepared by the present invention is crystal zinc silicate.
Fig. 2 is the luminescent spectrum figure of zinc silicate luminescent material prepared by embodiment 1, and as seen from Figure 2, the position of zinc silicate luminescent material emission peak prepared by the present invention is at 528nm, and its peak width at half height is 30.4nm.
Fig. 3 is the transmission electron microscope photo of zinc silicate luminescent material prepared by embodiment 1, and as seen from Figure 3, zinc silicate luminescent material particle diameter prepared by the present invention is greatly about about 15-20nm.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.

Claims (7)

1. utilize a method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material, it is characterized in that: the concrete steps of described method are as follows:
(1) by Zn (CH 3cOO) 22H 2o, Mn (NO 3) 24H 2o and cetyl trimethylammonium bromide are dissolved in deionized water, Zn (CH 3cOO) 22H 2o, Mn (NO 3) 24H 2the weight ratio of O and cetyl trimethylammonium bromide is 3-6:0.01-0.03:0.05, and the weightmeasurement ratio of cetyl trimethylammonium bromide and deionized water is 0.05:40-60g/ml, then adds waste silicon powder, waste silicon powder and Zn (CH 3cOO) 22H 2the weight ratio of O is 0.3-0.7:3-6, and stirring 15min, then adds sodium hydroxide or concentration is the ammoniacal liquor of 25%, stirs 10min, obtains mixing solutions;
(2) mixing solutions prepared by step (1) is put into the reactor that liner is tetrafluoroethylene, reactor is sealed, put into the baking oven reaction 12-48h that temperature is 130-200 DEG C, then room temperature is naturally cooled to after taking out, by product distilled water wash, centrifugation, obtains zinc silicate luminescent material after seasoning.
2. utilize the method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material as claimed in claim 1, it is characterized in that: in step (1), Zn (CH 3cOO) 22H 2o, Mn (NO 3) 24H 2the weight ratio of O and cetyl trimethylammonium bromide is 4.65:0.01:0.05.
3. utilize the method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material as claimed in claim 1, it is characterized in that: in step (1), the weightmeasurement ratio of cetyl trimethylammonium bromide and deionized water is 0.05:50g/ml.
4. utilize the method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material as claimed in claim 1, it is characterized in that: in step (1), waste silicon powder and Zn (CH 3cOO) 22H 2the weight ratio of O is 0.56:4.65.
5. utilize the method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material as claimed in claim 1, it is characterized in that: in step (1), the weight ratio of sodium hydroxide and cetyl trimethylammonium bromide is 0.01:0.05.
6. utilize the method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material as claimed in claim 1, it is characterized in that: in step (1), concentration is the ammoniacal liquor of 25% and the weight ratio of cetyl trimethylammonium bromide is 0.20:0.05.
7. utilize the method for waste silicon powder water heat transfer nanometer zinc silicate luminescent material as claimed in claim 1, it is characterized in that: in step (2), put into the baking oven reaction 48h that temperature is 130 DEG C.
CN201410306154.3A 2014-06-30 2014-06-30 A kind of method utilizing waste silicon powder water heat transfer nanometer zinc silicate luminescent material Expired - Fee Related CN104087289B (en)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
JPH0765038B2 (en) * 1987-02-10 1995-07-12 宇部興産株式会社 Manufacturing method of zinc silicate powder phosphor
CN1284108A (en) * 1997-12-04 2001-02-14 松下电器产业株式会社 Method of preparing high brightness, shorter persistence zinc orthosilicate phosphor
DE10111909A1 (en) * 2001-03-13 2002-09-26 Nonninger Ralph Production of nano-scale zinc silicate doped with manganese used as a luminescent pigment, comprises precursor formed by reacting an aqueous or aqueous/alcoholic solution with a base, and hydrothermally crystallizing the precursor
CN102502672A (en) * 2011-10-26 2012-06-20 中国科学院化学研究所 Layered multi-stage zinc silicate and preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0765038B2 (en) * 1987-02-10 1995-07-12 宇部興産株式会社 Manufacturing method of zinc silicate powder phosphor
CN1284108A (en) * 1997-12-04 2001-02-14 松下电器产业株式会社 Method of preparing high brightness, shorter persistence zinc orthosilicate phosphor
DE10111909A1 (en) * 2001-03-13 2002-09-26 Nonninger Ralph Production of nano-scale zinc silicate doped with manganese used as a luminescent pigment, comprises precursor formed by reacting an aqueous or aqueous/alcoholic solution with a base, and hydrothermally crystallizing the precursor
CN102502672A (en) * 2011-10-26 2012-06-20 中国科学院化学研究所 Layered multi-stage zinc silicate and preparation method and application thereof

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Title
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