CN101230268A - Method for preparing Mg doped ZnO luminescent material - Google Patents
Method for preparing Mg doped ZnO luminescent material Download PDFInfo
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- CN101230268A CN101230268A CNA2008100066592A CN200810006659A CN101230268A CN 101230268 A CN101230268 A CN 101230268A CN A2008100066592 A CNA2008100066592 A CN A2008100066592A CN 200810006659 A CN200810006659 A CN 200810006659A CN 101230268 A CN101230268 A CN 101230268A
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- zno luminescent
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Abstract
The invention relates to an Mg mixed ZnO luminescent material preparation method, which adopts coprecipitation to produce oxalate precursor of ZnC2O4 and MgC2O4, and obtains the Mg mixed ZnO luminescent material by roasting and decomposing the oxalate precursor. The invention can realize fine uniformity of the distribution of the Mg, precise chemical dosage proportions, lower trace impurity contents, and lower decomposition temperature. The preparation method of the invention is simple, can be operated easily, and is applicable for mass production. The prepared Mg mixed ZnO luminescent material has the advantages that the luminescent grains are even, the dispersibility is high, and the luminescent property is excellent. Under the irradiation of ultraviolet, the Mg mixed ZnO luminescent material can produce strong ultraviolet radiation as well as strong green ray, and can be used in LED, laser, and other fields by adjusting the content of the MG to change the bandwidth and the wavelength of the green ray.
Description
Technical field
The present invention relates to a kind of synthetic method of inorganic nano material, relate to the preparation method of the adulterated ZnO luminescent material of a kind of Mg specifically.
Background technology
Zinc oxide has purposes widely at aspects such as rubber, pottery, daily-use chemical industry, coating, magneticsubstances, can be used to make gas sensor, fluor, UV-preventing material, varistor, image recording material, pressure sensitive, piezoelectric, effective catalyst etc.Particularly, very extensive in field purposes such as photodiode, laser apparatus and optical communication devices as a kind of luminescent material.The luminosity of ZnO and bandwidth can be regulated by adding other metal ions, wherein the adulterated ZnO material of Mg can expand to 4.2eV from 3.3eV with bandwidth, and find at room temperature can produce bright UV luminous (Apply Physics Letter88 (2006) 023103), particularly recent findings Zn1-xMgxO bead can produce very strong orange-colored light (Nanotechmolgy.17 (2006) 973) down ultraviolet ray excited, so the adulterated ZnO luminescent material of Mg has tempting application prospect.The method for preparing at present the adulterated ZnO luminescent material of Mg has pulsed laser deposition, thermolysis process and sol-gel method, for example referring to Chinese patent application CN1715191A, CN1462822A and CN1542915A, but in order to realize that the good homogeneous of Mg in ZnO distributes, aforesaid method needs the preparation process or the expensive equipment of high relatively temperature, complexity.
Summary of the invention
The method that the purpose of this invention is to provide the adulterated ZnO luminescent material of a kind of Mg of preparation, this method is simple to operate, with low cost, is suitable for scale operation.Preparation process adopts the transient process that generates the oxalate presoma, adopt good homogeneity, exact chemical metering that coprecipitation process can realize the Mg dopant profiles than, lower trace impurity content and lower decomposition temperature, the uniform particles of preparation, good dispersity, have good luminosity, can be used for fields such as photodiode and laser apparatus.
The present invention is the zinc source with the zinc acetate, is the magnesium source with the magnesium acetate, and the oxalate presoma that adopts the roasting co-precipitation to generate prepares the adulterated ZnO luminescent material of Mg.
Detailed technology scheme of the present invention is as follows:
The adulterated ZnO luminescent material of a kind of Mg preparation method may further comprise the steps:
Step 1 adds zinc acetate in deionized water and magnesium acetate stirs until dissolving fully, gets the settled solution A of zinc acetate and magnesium acetate, wherein Zn
2+And Mg
2+Total concn be 0.1-0.5mol/L, and Mg
2+Molar weight be Zn
2+The 1.0-30.0% of molar weight;
Step 2 step 1 obtain zinc acetate and the settled solution A of magnesium acetate in add oxalic acid solution, the mole add-on of its mesoxalic acid is Zn
2+And Mg
2+The 1.1-1.5 of mole total amount doubly continues to stir 10-60 minute, forms white precipitate, filter, washing, 60-110 ℃ of oven dry, zinc oxide and magnesium oxide oxalate presoma ZnC
2O
2And MgC
2O
2, wherein the chemical reaction of Fa Shenging is:
Zn(Ac)
2+H
2C
2O
2→ZnC
2O
2+2HAc
Mg(Ac)2+H
2C
2O
2→MgC
2O
2+2HAc
Step 3 is with resulting zinc oxide of step 2 and magnesium oxide oxalate presoma ZnC
2O
2And MgC
2O
2At 500-950 ℃ of following roasting 0.5-3 hour, promptly get the adulterated ZnO luminescent material of Mg of the present invention,
The chemical reaction that takes place is:
ZnC
2O
2→ZnO+2CO
2
MgC
2O
2→MgO+2CO
2
Principle of the present invention is that the method that adopts co-precipitation to generate the oxalate presoma prepares the adulterated ZnO luminescent material of Mg, can realize the distribution of Mg good homogeneous in ZnO, excellent in chemical metering ratio, low trace impurity content and lower decomposition temperature, and good graininess.
The present invention compared with prior art has following advantage:
1, preparation cost of the present invention is cheap, method is simple, flow process is short, easy to operate, be suitable for scale operation.
2, the adulterated ZnO luminescent material of Mg of the present invention's preparation, the X-ray diffraction analysis proof has hexahedral Wurzite structure (as Fig. 1), owing to adopted the transient process of oxalate presoma, Mg is entrained in distribution good among the ZnO, excellent in chemical metering ratio, low trace impurity content and lower decomposition temperature can avoid occurring magnesian dephasign structure; And uniform particles (as Fig. 2), good dispersity.
3, the adulterated ZnO luminescent material of Mg of the present invention's preparation except having strong ultra-violet light-emitting, has also produced very strong green glow (as Fig. 3) under uviolizing, and can change its bandwidth and green wavelength by the content of regulating Mg.
Description of drawings
Fig. 1 is the X-ray diffractogram (the Mg molar content is 5.0%) of the adulterated ZnO luminescent material of Mg of the present invention's preparation
Fig. 2 is the transmission electron microscope photo (the Mg molar content is 5.0%) of the adulterated ZnO luminescent material of Mg of the present invention's preparation
Fig. 3 is the room temperature luminous spectrum of the adulterated ZnO luminescent material of Mg (the Mg molar content is 5.0%) under the 350nm wavelength excites of the present invention's preparation
Embodiment
Followingly specify the present invention, but the present invention is not limited to these embodiment according to embodiment.
Reagent used in the present invention is the AR level reagent that the Long Huagongshijichang of Chengdu section produces.
Embodiment 1
In the deionized water of 88ml, add 5.256g zinc acetate and 0.571g magnesium acetate and stir, get settled solution A until dissolving fully.Above-mentioned A solution adds the oxalic acid 100ml of 0.3mol/L, stirs 25 minutes, forms white precipitate.Filter, washing, 80 ℃ of oven dry get zinc oxide and magnesium oxide oxalate presoma white powder.Above-mentioned white powder 800 ℃ of following roastings 1 hour, is promptly got the adulterated ZnO luminescent material of Mg.Its median size of tem study is 500nm; The X-ray diffraction analysis proof has hexahedral Wurzite structure; Uv-visible absorption spectra shows that its energy of absorption edge is 380nm; Fluorescence spectrum shows that its green luminescence peak is at the 494nm place.
Embodiment 2
In the deionized water of 440ml, add 26.28g zinc acetate and 6.42g magnesium acetate and stir, get settled solution A until dissolving fully.Above-mentioned solution adds the oxalic acid 500ml of 0.3mol/L, stirs 30 minutes, forms white precipitate.Filter, washing, 90 ℃ of oven dry get zinc oxide and magnesium oxide oxalate presoma white powder.Above-mentioned white powder 800 ℃ of following roastings 2 hours, is promptly got the adulterated ZnO luminescent material of Mg.The X-ray diffraction analysis proof has hexahedral Wurzite structure; Uv-visible absorption spectra shows that its energy of absorption edge is 378nm; Fluorescence spectrum shows that its green luminescence peak is at the 476nm place.
Embodiment 3
In the deionized water of 88ml, add 5.256g zinc acetate and 0.052g magnesium acetate and stir, get settled solution A until dissolving fully.Above-mentioned solution adds the oxalic acid 95ml of 0.3mol/L, stirs 20 minutes, forms white precipitate.Filter, washing, 60 ℃ of oven dry get zinc oxide and magnesium oxide oxalate presoma white powder.Above-mentioned white powder 700 ℃ of following roastings 1 hour, is promptly got the adulterated ZnO luminescent material of Mg.The X-ray diffraction analysis proof has hexahedral Wurzite structure; Uv-visible absorption spectra shows that its energy of absorption edge is 382nm; Fluorescence spectrum shows that its green luminescence peak is at the 503nm place.
Embodiment 4
In the 440ml deionized water, add 26.28g zinc acetate and 4.53g magnesium acetate and stir, get settled solution A until dissolving fully.Above-mentioned solution adds the oxalic acid 750ml of 0.2mol/L, stirs 40 minutes, forms white precipitate.Filter, washing, 80 ℃ of oven dry get zinc oxide and magnesium oxide oxalate presoma white powder.Above-mentioned white powder 850 ℃ of following roastings 1.5 hours, is promptly got the adulterated ZnO luminescent material of Mg.The X-ray diffraction analysis proof has hexahedral Wurzite structure; Uv-visible absorption spectra shows that its energy of absorption edge is 379nm; Fluorescence spectrum shows that its green luminescence peak is at the 489nm place.
Claims (3)
1. the preparation method of the adulterated ZnO luminescent material of Mg is characterized in that comprising the steps:
Step 1: in deionized water, add zinc acetate and magnesium acetate and stir, get the settled solution A of zinc acetate and magnesium acetate, wherein Zn until dissolving fully
2+And Mg
2+Total concn be 0.1-0.5mol/L, and Mg
2+Molar weight be Zn
2+The 1.0-30.0% of molar weight;
Step 2: add oxalic acid solution in the settled solution A of the zinc acetate of step 1 and magnesium acetate, the mole add-on of its mesoxalic acid is Zn
2+And Mg
2+The 1.1-1.5 of mole total amount doubly continued to stir 10-60 minute, formed white precipitate and filtered, and washing 60-110 ℃ of oven dry, gets zinc oxide and magnesium oxide oxalate presoma ZnC
2O
4And MgC
2O
4
Step 3: with resulting zinc oxide of step 2 and magnesium oxide oxalate presoma ZnC
2O
4And MgC
2O
4At 500-950 ℃ of following roasting 0.5-3 hour, obtain the adulterated ZnO luminescent material of Mg.
2. the preparation method of the adulterated ZnO luminescent material of a kind of Mg as claimed in claim 1 is characterized in that adopting generation oxalate presoma ZnC
2O
4And MgC
2O
4Transient process.
3. the preparation method of the adulterated ZnO luminescent material of a kind of Mg as claimed in claim 1 is characterized in that adopting coprecipitation process to generate the oxalate presoma.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810006659A CN100587022C (en) | 2008-01-31 | 2008-01-31 | Method for preparing Mg doped ZnO luminescent material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810006659A CN100587022C (en) | 2008-01-31 | 2008-01-31 | Method for preparing Mg doped ZnO luminescent material |
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| Publication Number | Publication Date |
|---|---|
| CN101230268A true CN101230268A (en) | 2008-07-30 |
| CN100587022C CN100587022C (en) | 2010-02-03 |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941677A (en) * | 2010-08-31 | 2011-01-12 | 电子科技大学 | Method for preparing manganese oxide surface modified zinc oxide nano rod |
| CN102719249A (en) * | 2012-04-04 | 2012-10-10 | 河北联合大学 | Synthetic method of luminous ion doped zinc oxide microtube material |
-
2008
- 2008-01-31 CN CN200810006659A patent/CN100587022C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941677A (en) * | 2010-08-31 | 2011-01-12 | 电子科技大学 | Method for preparing manganese oxide surface modified zinc oxide nano rod |
| CN102719249A (en) * | 2012-04-04 | 2012-10-10 | 河北联合大学 | Synthetic method of luminous ion doped zinc oxide microtube material |
| CN102719249B (en) * | 2012-04-04 | 2014-02-12 | 河北联合大学 | Synthetic method of luminous ion doped zinc oxide microtube material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100587022C (en) | 2010-02-03 |
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