CN101439860A - Preparation of manganese-doped willemite yellow fluorescent powder - Google Patents
Preparation of manganese-doped willemite yellow fluorescent powder Download PDFInfo
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- CN101439860A CN101439860A CNA2008100723861A CN200810072386A CN101439860A CN 101439860 A CN101439860 A CN 101439860A CN A2008100723861 A CNA2008100723861 A CN A2008100723861A CN 200810072386 A CN200810072386 A CN 200810072386A CN 101439860 A CN101439860 A CN 101439860A
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Abstract
The invention relates to a preparation method for yellow fluorescent powder doped with manganese zinc silicate. The invention relates to a fluorescent powder, in particular to a method for preparing the yellow fluorescent powder doped with the manganese zinc silicate through the thermal reaction of low-temperature mixed solvent. The invention provides the method for preparing the yellow fluorescent powder doped with the manganese zinc silicate. The prepared yellow fluorescent powder doped with the manganese zinc silicate is characterized by small and even grain size, large specific surface area, stable performance, and the like. The chemical general expression is Zn2-xMnxSiO4, wherein x is more than or equal to 0.01 and less than or equal to 0.10. The method comprises the following steps: preparing an aqueous solution of zinc salt, manganese salt and sodium hydroxide; weighing nanometer silicon dioxide powder and the solution of zinc salt and manganese salt according to the stoichiometric ratio in the chemical general expression Zn2-xMnxSiO4, adding organic solvent, hydrazine hydrate and sodium hydroxide solution, and then dispersing the solution into suspension through ultrasonic wave; placing the suspension in a reaction kettle for reaction, and obtaining the yellow fluorescent powder doped with the manganese zinc silicate.
Description
Technical field
The present invention relates to a kind of fluorescent material, especially relate to a kind of employing low-temperature mixed solvent thermal reaction and prepare manganese-doped willemite (Zn
2SiO
4: the Mn) method of yellow fluorescent powder.
Background technology
According to the difference of synthesis condition zinc silicate (Zn as fluorescent material matrix
2SiO
4) there is different crystalline structure, as α-Zn
2SiO
4(JCPDS powdery diffractometry standard card number: 08-0492) be six side's phases, its cell parameter
,
γ=120 °; β-Zn
2SiO
4(JCPDS powdery diffractometry standard card number: 19-1479) belong to three monoclinic phases, its cell parameter
And α=89.99 °, β=96.98 °, γ=119.30 °.After mixing, the different zinc silicate of crystalline structure has different photoluminescent properties.Manganese-doped willemite (Zn with hexagonal system
2SiO
4: Mn) its fluorescence emission spectrum main peak is at 525nm, and it has advantages such as stable performance, luminous efficiency height and color and luster are pure as green emitting phosphor, is widely used in many-sides such as luminescent lamp, cathode tube, plasma flat-panel display and medical X-ray radiation detection.
The patent application of existing many relevant manganese-doped willemite green emitting phosphors, for example Chinese patent: 200410025310.9,200510038370.5,03126899.4,200710017267.1 and 200610023973.2 etc.Related preparation method comprises high temperature solid phase synthesis, wet chemical methods such as high temperature atomizing pyrolysis method, sol-gel method and low temperature co-precipitation.
Triclinic(crystalline)system manganese-doped willemite (β-Zn
2SiO
4: Mn) the fluorescence emission spectrum main peak between 560～575nm, jaundice look fluorescence, as a kind of effective yellow fluorescent powder, it is particularly important that its preparation process just seems.Its preparation method is detected in a small amount of scientific research document at present.Zinc nitrate, manganous nitrate and porous silicon are proposed 1050 ℃ of pyroreaction methods as (Nanotechnology 12 (2001) 547-551) such as (1) Goto; (2) Qian Yitai group (J.Lumin.121 (2006) 32-38) proposes with zinc chloride, Manganous chloride tetrahydrate, water glass and the sodium laurylsulfonate preparation method of rapid quenching behind 220 ℃ of heating 144h in the environment of second alcohol and water.Aforesaid method (1) is owing to need higher temperature, and sintering easily takes place the fluorescent material that obtains thus, and particle agglomeration, particle diameter is big and inhomogeneous.Need pulverize before using, process such as ball milling may cause the phosphor surface state to be destroyed, and influences fluorescence efficiency.In addition, raw material is as with solid-state mixing, causes the gathering of dopant ion easily and causes the self-priming cancellation.Aforesaid method (2) required time is long, and the purity of its yellow fluorescent powder often is subjected to the influence of quenching velocity, easily introduces the green fluorescence phase.Compare with above-mentioned manganese-doped willemite yellow fluorescent powder preparation method, the hot legal system of mixed solvent is equipped with fluorescent material, and it is low to have a preparation temperature, preparation time is short, uniform doping, advantages such as fluorescent powder size distribution unanimity are a kind of good methods of preparation manganese-doped willemite yellow fluorescent powder.
Summary of the invention
The object of the present invention is to provide a kind of employing mixed solvent thermal response, the manganese of realizing different concns easily mixes, and prepared manganese-doped willemite yellow fluorescent powder has the preparation method of the manganese-doped willemite yellow fluorescent powder of characteristics such as particle is little, particle diameter is even, specific surface area is big, stable performance.
Its chemical general formula of manganese-doped willemite yellow fluorescent powder of the present invention is: Zn
2-xMn
xSiO
4, 0.01≤x≤0.10 wherein.
Manganese-doped willemite yellow fluorescent powder particle little (reaching nanometer scale), be evenly distributed, stable chemical performance, colourity be pure, need not to pulverize, following process such as ball milling, can directly use.
The preparation method of manganese-doped willemite yellow fluorescent powder of the present invention may further comprise the steps:
1) zinc salt, manganese salt and sodium hydroxide water are mixed with solution;
2) press chemical general formula Zn
2-xMn
xSiO
4In stoichiometric ratio take by weighing silica nanometer powder, zinc salt and manganese salt solution, add organic solvent, hydrazine hydrate and sodium hydroxide solution after ultra-sonic dispersion become suspension;
3) suspension is placed reaction kettle for reaction, get manganese-doped willemite yellow fluorescent powder.
Zinc salt can be zinc nitrate, zinc acetate or zinc perchlorate etc. soluble in water contain the oxygen zinc salt, manganese salt can be that Manganous chloride tetrahydrate, manganous acetate or manganous carbonate etc. are water-soluble or be slightly soluble in the manganese salt of water.
In molar ratio, the consumption of sodium hydroxide and zinc salt is (1.0～1.5): 1.0, and the consumption of hydrazine hydrate and zinc salt is (5～12): 1.
Described organic solvent is preferably ethylene glycol, and by volume, the consumption of the organic solvent and the aqueous solution can be 8: (3～1), and the consumption of the organic solvent and the aqueous solution is preferably 8: 2; The temperature of reaction can be 180～220 ℃, and the time of reaction can be 48～120h.The temperature of reaction is preferably 200 ℃, and the time of reaction is preferably 72h.
The present invention has following outstanding advantage:
1) temperature of reaction is low, doping content variable (0.01～0.10mol%).
2) adopt method provided by the invention, silicon-dioxide is that nano powder is easy in organic solvent for ultrasonic dispersion, whole system can reach mixing of nano-scale, prepared manganese-doped willemite yellow fluorescent powder particle little (reaching nanometer scale), be evenly distributed, need not to pulverize, following process such as ball milling, can directly use.
3) adopt method provided by the invention, the stable chemical performance of prepared manganese-doped willemite yellow fluorescent powder, colourity is pure.
Description of drawings
Fig. 1 is the manganese-doped willemite yellow fluorescent powder (Zn that part is pressed the embodiment preparation
2-xMn
xSiO
4) the XRD diffractogram.In Fig. 1, X-coordinate be diffraction angle 2 θ (°), ordinate zou is diffracted intensity Intensity (a.u.).Curve a, b, c, d, e is corresponding embodiment 1,2,3,4,5 respectively.
Fig. 2 is the manganese-doped willemite yellow fluorescent powder (Zn by the present invention's preparation
2-xMn
xSiO
4) characteristic emission spectrum figure.In Fig. 2, X-coordinate is wavelength Wavelength (nm), and ordinate zou is diffracted intensity Intensity (a.u.).
Fig. 3 is the feature SEM figure of manganese-doped willemite yellow fluorescent powder.In Fig. 3, scale is 200nm.
Embodiment
A kind of preparation method of yellow fluorescent powder, its chemical constitution is: Zn
2-xMn
xSiO
40.01≤x≤0.10 wherein, its preparation process is to insert in the reactor behind the mixture ultra-sonic dispersion with silicon-dioxide, zinc nitrate solution, hydrazine hydrate solution, alkali lye, organic solvent and manganese salt solution to heat, and cooling back centrifugation, washing obtain the yellow fluorescent powder nano particle.
Embodiment 1
(1) with deionized water zinc nitrate, Manganous chloride tetrahydrate and sodium hydroxide are mixed with 1mol/L respectively, the aqueous solution of 1mol/L and 2mol/L.(2) calculate with silicon-dioxide consumption 1mmol, according to Zn
1.94SiO
4: Mn
0.06Stoichiometric ratio takes by weighing silicon-dioxide and measures zinc nitrate and manganese chloride solution.Zinc nitrate solution, manganese chloride solution, silicon-dioxide and ethylene glycol is ultrasonic mixed, drip hydrazine hydrate and sodium hydroxide solution again, wherein the consumption mol ratio of sodium hydroxide, hydrazine hydrate and zinc nitrate is 3:10:2, the consumption of the ethylene glycol and the aqueous solution is pressed 4:1 and is added, and the further ultra-sonic dispersion of said mixture becomes aaerosol solution.(3) suspension is transferred in the reactor, 200 ℃ of heating 72h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.94SiO
4: Mn
0.06Particle diameter 30～the 50nm of fluorescent material, excitation wavelength 245nm, emission wavelength 562nm, its XRD diffractogram is seen Fig. 1 (a).
(1) with deionized water zinc nitrate, Manganous chloride tetrahydrate and sodium hydroxide are mixed with 1mol/L respectively, the aqueous solution of 1mol/L and 2mol/L.(2) calculate with silicon-dioxide consumption 1mmol, according to Zn
1.86SiO
4: Mn
0.14Stoichiometric ratio takes by weighing silicon-dioxide and measures zinc nitrate and manganese chloride solution.Zinc nitrate solution, manganese chloride solution, silicon-dioxide and ethylene glycol is ultrasonic mixed, drip hydrazine hydrate and sodium hydroxide solution again, wherein the consumption mol ratio of sodium hydroxide, hydrazine hydrate and zinc nitrate is 3:10:2, the consumption of the ethylene glycol and the aqueous solution is pressed 4:1 and is added, and the further ultra-sonic dispersion of said mixture becomes aaerosol solution.(3) suspension is transferred in the reactor, 200 ℃ of heating 72h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.86SiO
4: Mn
0.14The particle diameter 40nm of fluorescent material, excitation wavelength 245nm, emission wavelength 562nm, its XRD diffractogram is seen Fig. 1 (b).
Embodiment 3
(1) with deionized water zinc nitrate, Manganous chloride tetrahydrate and sodium hydroxide are mixed with 1mol/L respectively, the aqueous solution of 1mol/L and 2mol/L.(2) calculate with silicon-dioxide consumption 1mmol, according to Zn
1.80SiO
4: Mn
0.20Stoichiometric ratio takes by weighing silicon-dioxide and measures zinc nitrate and manganese chloride solution.Zinc nitrate solution, manganese chloride solution, silicon-dioxide and ethylene glycol is ultrasonic mixed, drip hydrazine hydrate and sodium hydroxide solution again, wherein the consumption mol ratio of sodium hydroxide, hydrazine hydrate and zinc nitrate is 3:10:2, the consumption of the ethylene glycol and the aqueous solution is pressed 4:1 and is added, and the further ultra-sonic dispersion of said mixture becomes aaerosol solution.(3) suspension is transferred in the reactor, 200 ℃ of heating 72h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.80SiO
4: Mn
0.20The particle diameter 40nm of fluorescent material, excitation wavelength 245nm, emission wavelength 562nm, its XRD diffractogram is seen Fig. 1 (c).
Embodiment 4
(1) zinc nitrate and sodium hydroxide are mixed with the aqueous solution of 1mol/L and 2mol/L respectively with deionized water.(2) calculate with silicon-dioxide consumption 1mmol, according to Zn
1.94SiO
4: Mn
0.06Stoichiometric ratio takes by weighing silicon-dioxide and manganous carbonate and measures zinc nitrate solution.With zinc nitrate solution, manganous carbonate, silicon-dioxide and ethylene glycol is ultrasonic mixes, drip hydrazine hydrate and sodium hydroxide solution again, wherein the consumption mol ratio of sodium hydroxide, hydrazine hydrate and zinc nitrate is 3:20:2, the consumption of the ethylene glycol and the aqueous solution is pressed 4:1 and is added, and the said mixture ultra-sonic dispersion becomes aaerosol solution.(3) suspension is transferred in the reactor, 180 ℃ of heating 72h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.94SiO
4: Mn
0.06The particle diameter 30nm of fluorescent material, excitation wavelength 245nm, emission wavelength 563nm, its XRD diffractogram is seen Fig. 1 (d).
Embodiment 5
(1) zinc nitrate and sodium hydroxide are mixed with the aqueous solution of 1mol/L and 2mol/L respectively with deionized water.(2) calculate with silicon-dioxide consumption 1mmol, according to Zn
1.90SiO
4: Mn
0.10Stoichiometric ratio takes by weighing silicon-dioxide and manganese acetate and measures zinc nitrate solution.With zinc nitrate solution, manganese acetate, silicon-dioxide and ethylene glycol is ultrasonic mixes, drip hydrazine hydrate and sodium hydroxide solution again, wherein the consumption mol ratio of sodium hydroxide, hydrazine hydrate and zinc nitrate is 3:10:2, the consumption of the ethylene glycol and the aqueous solution is pressed 4:1 and is added, and the said mixture ultra-sonic dispersion becomes aaerosol solution.(3) suspension is transferred in the reactor, 220 ℃ of heating 48h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.90SiO
4: Mn
0.10The particle diameter 30nm of fluorescent material, excitation wavelength 245nm, emission wavelength 558nm.Fluorescent spectroscopy shows, contains a small amount of α-Zn in the product
2SiO
4: Mn, its XRD diffractogram is seen Fig. 1 (e).
Embodiment 6
(1) with deionized water zinc nitrate, Manganous chloride tetrahydrate and sodium hydroxide are mixed with 1mol/L respectively, the aqueous solution of 1mol/L and 2mol/L.(2) calculate with silicon-dioxide consumption 1mmol, according to Zn
1.94SiO
4: Mn
0.06Stoichiometric ratio takes by weighing silicon-dioxide and measures zinc nitrate and manganese chloride solution.Zinc nitrate solution, manganese chloride solution, silicon-dioxide and ethylene glycol is ultrasonic mixed, drip hydrazine hydrate and sodium hydroxide solution again, wherein the consumption mol ratio of sodium hydroxide, hydrazine hydrate and zinc nitrate is 2:10:2, the consumption of the ethylene glycol and the aqueous solution is pressed 8:2.5 and is added, and the further ultra-sonic dispersion of said mixture becomes aaerosol solution.(3) suspension is transferred in the reactor, 200 ℃ of heating 72h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.94SiO
4: Mn
0.06Particle diameter 30～the 50nm of fluorescent material, excitation wavelength 245nm, transmitted wave is about 562nm.
Embodiment 7
(1) with deionized water zinc nitrate, Manganous chloride tetrahydrate and sodium hydroxide are mixed with 1mol/L respectively, the aqueous solution of 1mol/L and 2mol/L.(2) calculate with silicon-dioxide consumption 1mmol, according to Zn
1.94SiO
4: Mn
0.06Stoichiometric ratio takes by weighing silicon-dioxide and measures zinc nitrate and manganese chloride solution.Zinc nitrate solution, manganese chloride solution, silicon-dioxide and ethylene glycol is ultrasonic mixed, drip hydrazine hydrate and sodium hydroxide solution again, wherein the consumption mol ratio of sodium hydroxide, hydrazine hydrate and zinc nitrate is 3:10:2, the consumption of the ethylene glycol and the aqueous solution is pressed 4:1 and is added, and the further ultra-sonic dispersion of said mixture becomes aaerosol solution.(3) suspension is transferred in the reactor, 200 ℃ of heating 120h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.94SiO
4: Mn
0.06Particle diameter 30～the 50nm of fluorescent material, excitation wavelength 245nm, transmitted wave is about 562nm.Reaction times is long, can cause yellow fluorescent powder impure, and XRD analysis shows individual green fluorescent material (α-Zn
1SiO
4: diffraction peak Mn) occurs.
(1) with deionized water zinc nitrate, Manganous chloride tetrahydrate and sodium hydroxide are mixed with 1mol/L respectively, the aqueous solution of 0.1mol/L and 2mol/L.(2) calculate with silicon-dioxide consumption 1mmol, according to Zn
1.94SiO
4: Mn
0.06Stoichiometric ratio takes by weighing silicon-dioxide and measures zinc nitrate and manganese chloride solution.Zinc nitrate solution, manganese chloride solution, silicon-dioxide and ethylene glycol is ultrasonic mixed, drip hydrazine hydrate and sodium hydroxide solution again, wherein the consumption mol ratio of sodium hydroxide, hydrazine hydrate and zinc nitrate is 2:17:2, the consumption of the ethylene glycol and the aqueous solution is pressed 8:2.2 and is added, and the further ultra-sonic dispersion of said mixture becomes aaerosol solution.(3) suspension is transferred in the reactor, 200 ℃ of heating 72h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.94SiO
4: Mn
0.06Particle diameter 30～the 50nm of fluorescent material, excitation wavelength 245nm, transmitted wave is about 562nm.
Fig. 2 provides the manganese-doped willemite yellow fluorescent powder (Zn by the present invention's preparation
2-xMn
xSiO
4) characteristic emission spectrum figure.
Fig. 3 provides the feature SEM figure of manganese-doped willemite yellow fluorescent powder.
Reference examples
(1) calculates with silicon-dioxide consumption 1mmol, according to Zn
1.94SiO
4: Mn
0.06Stoichiometric ratio takes by weighing silicon-dioxide, zinc nitrate and Manganous chloride tetrahydrate, according to sodium hydroxide and with 3: 2 weighing sodium hydroxide of zinc nitrate consumption mol ratio.Grind respectively and transfer in the reactor, add ethylene glycol 8ml and hydrazine hydrate solution 1ml (concentration 85%), the amount ratio of ethylene glycol and water reaches 8:0.15.The abundant ultra-sonic dispersion of said mixture becomes aaerosol solution.(2) suspension is transferred in the reactor, 200 ℃ of heating 72h.Cooling back water and washing with alcohol, air drying.Obtain yellow fluorescent powder Zn
1.94SiO
4: Mn
0.06XRD and sem analysis show that product is pure, but to compare degree of crystallinity poor with the previous embodiment product, and crystal grain is reunited serious.
Claims (9)
1. the preparation method of manganese-doped willemite yellow fluorescent powder, the chemical general formula that it is characterized in that described manganese-doped willemite yellow fluorescent powder is Zn
2-xMn
xSiO
4, 0.01≤x≤0.10 wherein;
The preparation method of described manganese-doped willemite yellow fluorescent powder may further comprise the steps:
1) zinc salt, manganese salt and sodium hydroxide water are mixed with solution;
2) press chemical general formula Zn
2-xMn
xSiO
4In stoichiometric ratio take by weighing silica nanometer powder, zinc salt and manganese salt solution, add organic solvent, hydrazine hydrate and sodium hydroxide solution after ultra-sonic dispersion become suspension;
3) suspension is placed reaction kettle for reaction, get manganese-doped willemite yellow fluorescent powder.
2. the preparation method of manganese-doped willemite yellow fluorescent powder as claimed in claim 1 is characterized in that zinc salt is zinc nitrate, zinc acetate or zinc perchlorate.
3. the preparation method of manganese-doped willemite yellow fluorescent powder as claimed in claim 1 is characterized in that manganese salt is Manganous chloride tetrahydrate, manganous acetate or manganous carbonate.
4. the preparation method of manganese-doped willemite yellow fluorescent powder as claimed in claim 1 is characterized in that in molar ratio, and the consumption of sodium hydroxide and zinc salt is 1.0～1.5: 1.0; The consumption of hydrazine hydrate and zinc salt is 5～12: 1.
5. the preparation method of manganese-doped willemite yellow fluorescent powder as claimed in claim 1 is characterized in that described organic solvent is an ethylene glycol.
6. the preparation method of manganese-doped willemite yellow fluorescent powder as claimed in claim 1 is characterized in that by volume, and the consumption of the organic solvent and the aqueous solution is 8: 3～1.
7. the preparation method of manganese-doped willemite yellow fluorescent powder as claimed in claim 6, the consumption that it is characterized in that the organic solvent and the aqueous solution is 8: 2.
8. the preparation method of manganese-doped willemite yellow fluorescent powder as claimed in claim 1 is characterized in that the temperature of reacting is 180～220 ℃, and the time of reaction is 48～120h.
9. the preparation method of manganese-doped willemite yellow fluorescent powder as claimed in claim 8 is characterized in that the temperature of reacting is 200 ℃, and the time of reaction is 72h.
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| CN102136405A (en) * | 2010-01-27 | 2011-07-27 | 海洋王照明科技股份有限公司 | Light-emitting element and manufacturing method and light-emitting method thereof |
| CN102660766A (en) * | 2012-05-08 | 2012-09-12 | 陕西科技大学 | Preparation method of Y2Si2O7 whisker |
| CN101671559B (en) * | 2009-09-19 | 2013-04-03 | 桂林理工大学 | Method for preparing M2SiO4-based fluorescent powders at lower temperature |
| CN103773363A (en) * | 2013-12-17 | 2014-05-07 | 中国计量学院 | Green manganese-activated zinc silicate fluorescent powder and preparation method thereof |
| CN109824055A (en) * | 2019-04-04 | 2019-05-31 | 河北工业大学 | The method for preparing nano-sheet zinc silicate compound adsorbent using iron tailings |
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2008
- 2008-12-15 CN CN2008100723861A patent/CN101439860B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101671559B (en) * | 2009-09-19 | 2013-04-03 | 桂林理工大学 | Method for preparing M2SiO4-based fluorescent powders at lower temperature |
| CN102136405A (en) * | 2010-01-27 | 2011-07-27 | 海洋王照明科技股份有限公司 | Light-emitting element and manufacturing method and light-emitting method thereof |
| CN102660766A (en) * | 2012-05-08 | 2012-09-12 | 陕西科技大学 | Preparation method of Y2Si2O7 whisker |
| CN102660766B (en) * | 2012-05-08 | 2015-02-25 | 陕西科技大学 | Preparation method of Y2Si2O7 whisker |
| CN103773363A (en) * | 2013-12-17 | 2014-05-07 | 中国计量学院 | Green manganese-activated zinc silicate fluorescent powder and preparation method thereof |
| CN109824055A (en) * | 2019-04-04 | 2019-05-31 | 河北工业大学 | The method for preparing nano-sheet zinc silicate compound adsorbent using iron tailings |
| CN109824055B (en) * | 2019-04-04 | 2022-06-07 | 河北工业大学 | Method for preparing nano flaky zinc silicate composite adsorbent by using iron tailings |
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