CN101629079A - Method for preparing green luminescent material of yttrium zirconate doped with terbium - Google Patents
Method for preparing green luminescent material of yttrium zirconate doped with terbium Download PDFInfo
- Publication number
- CN101629079A CN101629079A CN 200910102148 CN200910102148A CN101629079A CN 101629079 A CN101629079 A CN 101629079A CN 200910102148 CN200910102148 CN 200910102148 CN 200910102148 A CN200910102148 A CN 200910102148A CN 101629079 A CN101629079 A CN 101629079A
- Authority
- CN
- China
- Prior art keywords
- terbium
- solution
- luminescent material
- yttrium
- green luminescent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000463 material Substances 0.000 title claims abstract description 20
- 229910052771 Terbium Inorganic materials 0.000 title claims abstract description 19
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 17
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 20
- YJVUGDIORBKPLC-UHFFFAOYSA-N terbium(3+);trinitrate Chemical compound [Tb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YJVUGDIORBKPLC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- -1 rare earth cation Chemical class 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 3
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 claims description 15
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 abstract description 9
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 238000011049 filling Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 9
- 150000002910 rare earth metals Chemical class 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 7
- 238000005424 photoluminescence Methods 0.000 description 6
- 238000000295 emission spectrum Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012720 thermal barrier coating Substances 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
Images
Landscapes
- Luminescent Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing a green luminescent material of yttrium zirconate doped with terbium. The method comprises the following steps: dissolving yttrium nitrate and terbium nitrate in deionized water according to the mole ratio and stirring; adding zirconium oxychloride with equal molar weight with the total rare earth cation into the solution and fully stirring; adding a sodium hydroxide solution drops by drops to obtain a white precipitate and controlling the pH value of the solution at 7-9; putting the solution into a high-pressure kettle, taking the filling degree at 80% and processing for 6-40 hours at 180-220 DEG C; and finally, centrifugalizing and drying the processed solution to obtain the green luminescent material of yttrium zirconate doped with terbium. The invention adopts a hydrothermal method to realize the synthesis of the green luminescent material of yttrium zirconate doped with terbium and has better crystallization performance of a product, simple technological process and mild condition.
Description
Technical field
The present invention relates to a kind of preparation method of green luminescent material of yttrium zirconate doped with terbium.
Background technology
Rare earth zirconate (Re
2Zr
2O
7) purposes is very extensive, and have a lot of special performances, as high-melting-point, macroion electroconductibility, high chemical stability, high catalytic activity etc.It is widely used as thermal barrier coating in recent years, owing to very low thermal conductivity, higher chemical stability, thereby receives much concern.Rare earth zirconate still is a kind of good catalyzer, is widely used in catalytic fields such as photochemical catalysis.In recent years, its matrix as embedded photoluminescent material comes into one's own, but correlative study is also less.
Existing research report about rare earth zirconic acid yttrium material mainly concentrates on thermal barrier coating and photochemical catalysis aspect, its preparation method is relatively single, be mainly high temperature solid-phase sintering method and sol-gel method [Aiyu Zhang, etal, Systematic research on RE
2Zr
2O7 (RE=La, Nd, Eu and Y) nanocrystals:Preparation, structure and photoluminescence characterization, Solid State Sciences, 10 (2008) 74-81], almost do not have about hydrothermal method synthetic report.In addition, the zirconic acid yttrium is also considerably less as the report of luminescent material matrix research, the synthetic report that yet there are no of green luminescent material of yttrium zirconate doped with terbium.
Summary of the invention
The object of the present invention is to provide a kind of yttrium zirconate doped with terbium (Y
2Zr
2O
7: Tb
3+) preparation method of green luminescent material.Adopt hydro-thermal technology, under lower temperature of reaction, realized the preparation of green luminescent material of yttrium zirconate doped with terbium.
The step of the technical solution used in the present invention is as follows:
1) Yttrium trinitrate, Terbium trinitrate are dissolved in the deionized water by mole per-cent, the ratio of control Terbium trinitrate is 4%～7% of a total rare earth cation mole number, stirs;
2) basic zirconium chloride of mole numbers such as adding and above-mentioned total rare earth cation in above-mentioned solution stirs;
3) sodium hydroxide solution that dropwise adds 1.0 mol generates white precipitate, and the pH value of control solution is 7～9, continues stirring;
4) above-mentioned solution is packed into autoclave adopts hydro-thermal technology, and the solution centrifugal of handling well, drying obtain green luminescent material of yttrium zirconate doped with terbium.
Described hydro-thermal technology, temperature are controlled to be 180～220 ℃, and the treatment time is 6～40 hours.
The beneficial effect that the present invention has is:
The present invention is to be reactant with Yttrium trinitrate, Terbium trinitrate, basic zirconium chloride, has synthesized green luminescent material of yttrium zirconate doped with terbium by hydro-thermal technology.The product crystallinity is better, and preparation technology is simple, and the reaction conditions gentleness is significant to exploring the development of new rare earth luminescent material, will expand new field for the research of rare earth luminescent material simultaneously.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 products therefrom.
Curve (a) and (b), (c), (d) corresponding embodiment 1,2,3 of difference and 4 products therefrom photoluminescence emmission spectrum spectrograms among Fig. 2.
Embodiment
Embodiment 1:
Get 1.1490 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.0715 gram Terbium trinitrate (Tb (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the volumetric molar concentration of Yttrium trinitrate, Terbium trinitrate is respectively 0.0750 mol, 0.0039 mol, stirs 20 minutes; Get basic zirconium chloride (ZrOCl
28H
2O) 1.0180 grams are dissolved in 40 ml deionized water, and the volumetric molar concentration of basic zirconium chloride is 0.0789 mol, stirs 20 minutes.Zirconium oxychloride solution is dropwise splashed in the mixing solutions of above-mentioned Yttrium trinitrate and Terbium trinitrate, stirred 15 minutes.Dropwise add the sodium hydroxide solution of 1 mol in above-mentioned mixing solutions, the pH value of regulator solution is 7.0, continues to stir 0.5 hour.The above-mentioned solution for preparing is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 20 hours down at 180 ℃, the solution centrifugal of handling well, drying, obtained required product, and wherein the doping content of terbium accounts for 5% of total rare earth total mole number.Fig. 1 is the XRD figure spectrum of this routine products therefrom, [M.Kumar, et al, Electrical and sintering behaviour of Y in each diffractive features peak position and the document among the figure
2Zr
2O
7(YZ) pyrochlore-based materials-theinfluence of bismuth, Materials Chemistry and Physics, 92 (2005) 295-302] described Y
2Zr
2O
7Characteristic peaks good correspondence is arranged, the variation that does not obviously cause structure of mixing of terbium is described.Curve among Fig. 2 (a) is its photoluminescence emmission spectrum, has sharp-pointed green emission spectrum in 545 nanometers.
Embodiment 2:
Get 1.7240 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.1301 gram Terbium trinitrate (Tb (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the volumetric molar concentration of Yttrium trinitrate, Terbium trinitrate is respectively 0.1125 mol, 0.0072 mol, stirs 10 minutes; Get basic zirconium chloride (ZrOCl
28H
2O) 1.5427 grams are dissolved in 40 ml deionized water, and the volumetric molar concentration of basic zirconium chloride is 0.1197 mol, stirs 20 minutes.Zirconium oxychloride solution is dropwise splashed in the mixing solutions of above-mentioned Yttrium trinitrate and Terbium trinitrate, stirred 20 minutes.Dropwise add the sodium hydroxide solution of 1 mol in above-mentioned mixing solutions, the pH value of regulator solution is 8.0, continues to stir 0.5 hour.The above-mentioned solution for preparing is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 10 hours down at 200 ℃, the solution centrifugal of handling well, drying, obtained required product, and the doping content of terbium accounts for 6% of total rare earth total mole number.Curve among Fig. 2 (b) is its photoluminescence emmission spectrum, has sharp-pointed green emission spectrum in 545 nanometers.
Embodiment 3:
Get 2.2980 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.2046 gram Terbium trinitrate (Tb (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the volumetric molar concentration of Yttrium trinitrate, Terbium trinitrate is respectively 0.15 mol, 0.0113 mol, stirs 20 minutes; Get basic zirconium chloride (ZrOCl
28H
2O) 2.0790 grams are dissolved in 40 ml deionized water, and the volumetric molar concentration of basic zirconium chloride is 0.1613 mol, stirs 15 minutes.Zirconium oxychloride solution is dropwise splashed in the mixing solutions of above-mentioned Yttrium trinitrate and Terbium trinitrate, stirred 20 minutes.Dropwise add the sodium hydroxide solution of 1 mol in above-mentioned mixing solutions, the pH value of regulator solution is 9.0, continues to stir 0.5 hour.The above-mentioned solution for preparing is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 40 hours down at 180 ℃, the solution centrifugal of handling well, drying, obtained required product, and the doping content of terbium accounts for 7% of total rare earth total mole number.Curve among Fig. 2 (c) is its photoluminescence emmission spectrum, has sharp-pointed green emission spectrum in 545 nanometers.
Embodiment 4:
Get 3.4470 gram Yttrium trinitrate (Y (NO respectively
3)
36H
2O), 0.1699 gram Terbium trinitrate (Tb (NO
3)
36H
2O) be dissolved in 40 ml deionized water, the volumetric molar concentration of Yttrium trinitrate, Terbium trinitrate is respectively 0.2250 mol, 0.0094 mol, stirs 20 minutes; Get basic zirconium chloride (ZrOCl
28H
2O) 3.0211 grams are dissolved in 40 ml deionized water, and the volumetric molar concentration of basic zirconium chloride is 0.2344 mol, stirs 15 minutes.Zirconium oxychloride solution is dropwise splashed in the mixing solutions of above-mentioned Yttrium trinitrate and Terbium trinitrate, stirred 20 minutes.Dropwise add the sodium hydroxide solution of 1 mol in above-mentioned mixing solutions, the pH value of regulator solution is 9.0, continues to stir 0.5 hour.The above-mentioned solution for preparing is put into the teflon-lined autoclave, and compactedness is 80%, and the liner volume is 100 milliliters.This solution was handled 6 hours down at 220 ℃, the solution centrifugal of handling well, drying, obtained required product, and the doping content of terbium accounts for 4% of total rare earth total mole number.Curve among Fig. 2 (d) is its photoluminescence emmission spectrum, has sharp-pointed green emission spectrum in 545 nanometers.
Claims (2)
1, a kind of preparation method of green luminescent material of yttrium zirconate doped with terbium is characterized in that the step of this method is as follows:
1) Yttrium trinitrate, Terbium trinitrate are dissolved in the deionized water by mole per-cent, the ratio of control Terbium trinitrate is 4%～7% of a total rare earth cation mole number, stirs;
2) basic zirconium chloride of mole numbers such as adding and above-mentioned total rare earth cation in above-mentioned solution stirs;
3) sodium hydroxide solution that dropwise adds 1.0 mol generates white precipitate, and the pH value of control solution is 7～9, continues stirring;
4) above-mentioned solution is packed into autoclave adopts hydro-thermal technology, and the solution centrifugal of handling well, drying obtain green luminescent material of yttrium zirconate doped with terbium.
2, the preparation method of a kind of green luminescent material of yttrium zirconate doped with terbium according to claim 1 is characterized in that: described hydro-thermal technology, temperature are controlled to be 180～220 ℃, and the treatment time is 6～40 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910102148 CN101629079B (en) | 2009-08-17 | 2009-08-17 | Method for preparing green luminescent material of yttrium zirconate doped with terbium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910102148 CN101629079B (en) | 2009-08-17 | 2009-08-17 | Method for preparing green luminescent material of yttrium zirconate doped with terbium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101629079A true CN101629079A (en) | 2010-01-20 |
| CN101629079B CN101629079B (en) | 2012-12-26 |
Family
ID=41574363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910102148 Expired - Fee Related CN101629079B (en) | 2009-08-17 | 2009-08-17 | Method for preparing green luminescent material of yttrium zirconate doped with terbium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101629079B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824320A (en) * | 2010-05-19 | 2010-09-08 | 北京大学 | Red fluorescent powder, preparation method and application thereof |
| CN105801114A (en) * | 2014-12-29 | 2016-07-27 | 中国科学院上海硅酸盐研究所 | Method for preparing ultrafine-yttria stable zirconia powder |
| CN115820246A (en) * | 2022-11-21 | 2023-03-21 | 桂林电子科技大学 | Preparation method and application of rare earth terbium-doped gallium oxide fluorescent material |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5518830A (en) * | 1995-05-12 | 1996-05-21 | The Trustees Of The University Of Pennsylvania | Single-component solid oxide bodies |
| CN1239673C (en) * | 2003-10-23 | 2006-02-01 | 北京有色金属研究总院 | Red luminescent powder in use for LED, preparing method and electric light source produced |
| CN1331982C (en) * | 2004-10-11 | 2007-08-15 | 北京有色金属研究总院 | Phosphor powder of composite oxide in use for white light LED and fabricated electric light source |
-
2009
- 2009-08-17 CN CN 200910102148 patent/CN101629079B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824320A (en) * | 2010-05-19 | 2010-09-08 | 北京大学 | Red fluorescent powder, preparation method and application thereof |
| CN105801114A (en) * | 2014-12-29 | 2016-07-27 | 中国科学院上海硅酸盐研究所 | Method for preparing ultrafine-yttria stable zirconia powder |
| CN115820246A (en) * | 2022-11-21 | 2023-03-21 | 桂林电子科技大学 | Preparation method and application of rare earth terbium-doped gallium oxide fluorescent material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101629079B (en) | 2012-12-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100462305C (en) | Universal synthesizing method for lanthanide series rare earth stannate nano powder | |
| CN108383160B (en) | Preparation method and application of metal element doped BiOCl nanosheet material | |
| Narendar et al. | Synthesis, decomposition and crystallization characteristics of peroxo− citrato− niobium: an aqueous niobium precursor | |
| CN101629078B (en) | Method for preparing cubic shape green luminescent material of lanthanum zirconate doped with cerium and terbium | |
| CN107855130A (en) | A kind of solar energy fixed nitrogen photochemical catalyst and application thereof and preparation method | |
| CN101629079B (en) | Method for preparing green luminescent material of yttrium zirconate doped with terbium | |
| CN102888222A (en) | Solvothermal preparation method of yellow luminous nanometer upconversion material | |
| CN104528799B (en) | A kind of preparation method of magnesio rare earth hexa-aluminate superfine powder | |
| CN102277162A (en) | Europium-doped hydrated zinc molybdate high-efficient red fluorescent powder and preparation method thereof | |
| CN101671558B (en) | Preparation method of dysprosium zirconate terbium-doped green luminescent material | |
| Lin et al. | Effects of multiple irradiations on luminescent materials and energy savings–A case study for the synthesis of BaMO4: Ln3+ (M= W, Mo; Ln= Eu, Tb) phosphors | |
| CN104108737B (en) | The synthetic method of copper-rare earth nano petal-shaped metal-oxide | |
| CN107400510A (en) | A kind of plant growth lamp high light-effect rare earth ion terbium europium codope bismuth phosphate red fluorescence powder and preparation method thereof | |
| CN114540935B (en) | Rare earth praseodymium borate crystal material and preparation method thereof | |
| Adcock et al. | Bismuth (III)-thiophenedicarboxylates as host frameworks for lanthanide ions: synthesis, structural characterization, and photoluminescent behavior | |
| CN101619212B (en) | Carbonic acid lanthana based nanometer fluorescence power and preparation method thereof | |
| CN101376520B (en) | Method for preparing Ce3+ doped lutetium oxyorthosilicate luminescent powder using organic compound auxiliary low temperature | |
| CN105038785A (en) | (SrxCay)0.97TiO3:Eu3+0.03 fluorescent powder and preparing method thereof | |
| CN112340773B (en) | Preparation method of nano zirconia luminescent material | |
| CN102745747B (en) | Preparation method for rod-like Sc2W3O12 negative thermal expansion material | |
| CN101591538A (en) | A kind of rare-earth phosphate LnPO 4: the preparation method of Eu red fluorescence powder | |
| CN101693520B (en) | Industrialized process for preparing cerium oxide nano-rods doped with rare earth elements | |
| CN107335420B (en) | A kind of nano wire reticular structure calcium titanate visible light catalyst and its preparation method and application | |
| CN102559182A (en) | Novel white-light nano-luminescent material of yttrium aluminate activated by dysprosium | |
| CN102533247B (en) | A kind of containing dysprosium fluorescent crystal and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121226 Termination date: 20130817 |